Separation of aromatic carboxylic acids using quaternary ammonium salts on reversed-phase HPLC. 2. Application for the analysis of Loy Yang coal oxidation products

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kawamura, K.; Okuwaki, A.; Verheyen, T.V.

In order to develop separation processes and analytical methods for aromatic carboxylic acids for the coal oxidation products, the separation behavior of aromatic carboxylic acids on a reversed-phase HPLC using eluent containing quaternary ammonium salt was optimized using the solvent gradient method. This method was applied for the analysis of Loy Yang coal oxidation products. It was confirmed that the analytical data using this method were consistent with those determined using gas chromatography.

Macro-fingerprint analysis-through-separation of licorice based on FT-IR and 2DCOS-IR

NASA Astrophysics Data System (ADS)

Wang, Yang; Wang, Ping; Xu, Changhua; Yang, Yan; Li, Jin; Chen, Tao; Li, Zheng; Cui, Weili; Zhou, Qun; Sun, Suqin; Li, Huifen

2014-07-01

In this paper, a step-by-step analysis-through-separation method under the navigation of multi-step IR macro-fingerprint (FT-IR integrated with second derivative IR (SD-IR) and 2DCOS-IR) was developed for comprehensively characterizing the hierarchical chemical fingerprints of licorice from entirety to single active components. Subsequently, the chemical profile variation rules of three parts (flavonoids, saponins and saccharides) in the separation process were holistically revealed and the number of matching peaks and correlation coefficients with standards of pure compounds was increasing along the extracting directions. The findings were supported by UPLC results and a verification experiment of aqueous separation process. It has been demonstrated that the developed multi-step IR macro-fingerprint analysis-through-separation approach could be a rapid, effective and integrated method not only for objectively providing comprehensive chemical characterization of licorice and all its separated parts, but also for rapidly revealing the global enrichment trend of the active components in licorice separation process.

SEPHYDRO: An Integrated Multi-Filter Web-Based Tool for Baseflow Separation

NASA Astrophysics Data System (ADS)

Serban, D.; MacQuarrie, K. T. B.; Popa, A.

2017-12-01

Knowledge of baseflow contributions to streamflow is important for understanding watershed scale hydrology, including groundwater-surface water interactions, impact of geology and landforms on baseflow, estimation of groundwater recharge rates, etc. Baseflow (or hydrograph) separation methods can be used as supporting tools in many areas of environmental research, such as the assessment of the impact of agricultural practices, urbanization and climate change on surface water and groundwater. Over the past few decades various digital filtering and graphically-based methods have been developed in an attempt to improve the assessment of the dynamics of the various sources of streamflow (e.g. groundwater, surface runoff, subsurface flow); however, these methods are not available under an integrated platform and, individually, often require significant effort for implementation. Here we introduce SEPHYDRO, an open access, customizable web-based tool, which integrates 11 algorithms allowing for separation of streamflow hydrographs. The streamlined interface incorporates a reference guide as well as additional information that allows users to import their own data, customize the algorithms, and compare, visualise and export results. The tool includes one-, two- and three-parameter digital filters as well as graphical separation methods and has been successfully applied in Atlantic Canada, in studies dealing with nutrient loading to fresh water and coastal water ecosystems. Future developments include integration of additional separation algorithms as well as incorporation of geochemical separation methods. SEPHYDRO has been developed through a collaborative research effort between the Canadian Rivers Institute, University of New Brunswick (Fredericton, New Brunswick, Canada), Agriculture and Agri-Food Canada and Environment and Climate Change Canada and is currently available at http://canadianriversinstitute.com/tool/

Identification of inorganic ions in post-blast explosive residues using portable CE instrumentation and capacitively coupled contactless conductivity detection.

PubMed

Hutchinson, Joseph P; Johns, Cameron; Breadmore, Michael C; Hilder, Emily F; Guijt, Rosanne M; Lennard, Chris; Dicinoski, Greg; Haddad, Paul R

2008-11-01

Novel CE methods have been developed on portable instrumentation adapted to accommodate a capacitively coupled contactless conductivity detector for the separation and sensitive detection of inorganic anions and cations in post-blast explosive residues from homemade inorganic explosive devices. The methods presented combine sensitivity and speed of analysis for the wide range of inorganic ions used in this study. Separate methods were employed for the separation of anions and cations. The anion separation method utilised a low conductivity 70 mM Tris/70 mM CHES aqueous electrolyte (pH 8.6) with a 90 cm capillary coated with hexadimethrine bromide to reverse the EOF. Fifteen anions could be baseline separated in 7 min with detection limits in the range 27-240 microg/L. A selection of ten anions deemed most important in this application could be separated in 45 s on a shorter capillary (30.6 cm) using the same electrolyte. The cation separation method was performed on a 73 cm length of fused-silica capillary using an electrolyte system composed of 10 mM histidine and 50 mM acetic acid, at pH 4.2. The addition of the complexants, 1 mM hydroxyisobutyric acid and 0.7 mM 18-crown-6 ether, enhanced selectivity and allowed the separation of eleven inorganic cations in under 7 min with detection limits in the range 31-240 microg/L. The developed methods were successfully field tested on post-blast residues obtained from the controlled detonation of homemade explosive devices. Results were verified using ion chromatographic analyses of the same samples.

Optimized anion exchange column isolation of zirconium-89 ( 89 Zr) from yttrium cyclotron target: Method development and implementation on an automated fluidic platform

DOE Office of Scientific and Technical Information (OSTI.GOV)

O’Hara, Matthew J.; Murray, Nathaniel J.; Carter, Jennifer C.

Zirconium-89 (89Zr), produced by the (p,n) reaction from naturally monoisotopic yttrium (natY), is a promising positron emitting isotope for immunoPET imaging. Its long half-life of 78.4 h is sufficient for evaluating slow physiological processes. A prototype automated fluidic system, coupled to on-line and in-line detectors, has been constructed to facilitate development of new 89Zr purification methodologies. The highly reproducible reagent delivery platform and near-real time monitoring of column effluents allows for efficient method optimization. The separation of Zr from dissolved Y metal targets was evaluated using several anion exchange resins. Each resin was evaluated against its ability to quantitatively capturemore » Zr from a load solution that is high in dissolved Y. The most appropriate anion exchange resin for this application was identified, and the separation method was optimized. The method is capable of a high Y decontamination factor (>105) and has been shown to separate Fe, an abundant contaminant in Y foils, from the 89Zr elution fraction. Finally, the performance of the method was evaluated using cyclotron bombarded Y foil targets. The separation method was shown to achieve >95% recovery of the 89Zr present in the foils. The 89Zr eluent, however, was in a chemical matrix not immediately conducive to labeling onto proteins. The main intent of this study was to develop a tandem column 89Zr purification process, wherein the anion exchange column method described here is the first separation in a dual-column purification process.« less

Final Report: Computer Simulation of Osmosis and Reverse Osmosis in Structured Membranes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sohail Murad

2012-01-03

Molecular simulation methods were developed as part of this project to increase our fundamental understanding of membrane based separation systems. Our simulations clarified for example that steric (size) effects had a significant impact on the desalination membranes. Previously it was thought the separation was entirely driven by coulombic force (attractive/repulsive forces at the membrane surfaces). Steric effects played an important role, because salt ions in brackish water are never present alone, but are strongly hydrated which effectively increases their size, and makes it impossible to enter a membrane, while the smaller water molecules can enter more readily. Membrane surface effectsmore » did play a role in increasing the flux of water, but not in the separation itself. In addition we also developed simulation methods to study ion exchange, gas separations, and pervaporation. The methods developed were used to once again increase our fundamental understanding of these separation processes. For example our studies showed that when the separation factor of gases in membranes can be significantly affected by the presence of another gas, it is generally because the separation mechanism has changed. For example in the case of nitrogen and carbon dioxide, in their pure state the separation factor is determined by diffusion, while in mixtures it is influenced more by adsorption in the membrane (zeolite in our case) Finally we developed a new technique using the NMR chemical shift to determine intermolecular interactions for mixtures. For polar-nonpolar systems such as Xe dissolved in water we were able to significantly improve the accuracy of gas solubilities, which are very sensitive to the cross interaction between water and Xe.« less

Numerical techniques for the solution of the compressible Navier-Stokes equations and implementation of turbulence models. [separated turbulent boundary layer flow problems

NASA Technical Reports Server (NTRS)

Baldwin, B. S.; Maccormack, R. W.; Deiwert, G. S.

1975-01-01

The time-splitting explicit numerical method of MacCormack is applied to separated turbulent boundary layer flow problems. Modifications of this basic method are developed to counter difficulties associated with complicated geometry and severe numerical resolution requirements of turbulence model equations. The accuracy of solutions is investigated by comparison with exact solutions for several simple cases. Procedures are developed for modifying the basic method to improve the accuracy. Numerical solutions of high-Reynolds-number separated flows over an airfoil and shock-separated flows over a flat plate are obtained. A simple mixing length model of turbulence is used for the transonic flow past an airfoil. A nonorthogonal mesh of arbitrary configuration facilitates the description of the flow field. For the simpler geometry associated with the flat plate, a rectangular mesh is used, and solutions are obtained based on a two-equation differential model of turbulence.

Separation behavior of boundary layers on three-dimensional wings

NASA Technical Reports Server (NTRS)

Stock, H. W.

1981-01-01

An inverse boundary layer procedure for calculating separated, turbulent boundary layers at infinitely long, crabbing wing was developed. The procedure was developed for calculating three dimensional, incompressible turbulent boundary layers was expanded to adiabatic, compressible flows. Example calculations with transsonic wings were made including viscose effects. In this case an approximated calculation method described for areas of separated, turbulent boundary layers, permitting calculation of this displacement thickness. The laminar boundary layer development was calculated with inclined ellipsoids.

Optimization of a reversed-phase-high-performance thin-layer chromatography method for the separation of isoniazid, ethambutol, rifampicin and pyrazinamide in fixed-dose combination antituberculosis tablets.

PubMed

Shewiyo, D H; Kaale, E; Risha, P G; Dejaegher, B; Smeyers-Verbeke, J; Vander Heyden, Y

2012-10-19

This paper presents the development of a new RP-HPTLC method for the separation of pyrazinamide, isoniazid, rifampicin and ethambutol in a four fixed-dose combination (4 FDC) tablet formulation. It is a single method with two steps in which after plate development pyrazinamide, isoniazid and rifampicin are detected at an UV wavelength of 280 nm. Then ethambutol is derivatized and detected at a VIS wavelength of 450 nm. Methanol, ethanol and propan-1-ol were evaluated modifiers to form alcohol-water mobile phases. Systematic optimization of the composition of each alcohol in the mobile phase was carried out using the window diagramming concept to obtain the best separation. Examination of the Rf distribution of the separated compounds showed that separation of the compounds with the mobile phase containing ethanol at the optimal fraction was almost situated within the optimal Rf-values region of 0.20-0.80. Therefore, ethanol was selected as organic modifier and the optimal mobile phase composition was found to be ethanol, water, glacial acetic acid (>99% acetic acid) and 37% ammonia solution (70/30/5/1, v/v/v/v). The method is new, quick and cheap compared to the actual method in the International Pharmacopoeia for the assay of the 4 FDC tablets, which involves the use of two separate HPLC methods. Copyright © 2012 Elsevier B.V. All rights reserved.

Comparison of chiral electrophoretic separation methods for phenethylamines and application on impurity analysis.

PubMed

Borst, Claudia; Holzgrabe, Ulrike

2010-12-15

A chiral microemulsion electrokinetic chromatography method has been developed for the separation of the enantiomers of the phenethylamines ephedrine, N-methylephedrine, norephedrine, pseudoephedrine, adrenaline (epinephrine), 2-amino-1-phenylethanol, diethylnorephedrine, and 2-(dibutylamino)-1-phenyl-1-propanol, respectively. The separations were achieved using an oil-in-water microemulsion consisting of the oil-component ethyl acetate, the surfactant sodium dodecylsulfate, the cosurfactant 1-butanol, the organic modifier propan-2-ol and 20mM phosphate buffer pH 2.5 as aqueous phase. For enantioseparation sulfated beta-cyclodextrin was added. The method was compared to an already described CZE method, which made use of heptakis(2,3-di-O-diacetyl-6-O-sulfo)-beta-cyclodextrin (HDAS) as chiral selector. Additionally, the developed method was successfully applied to the related substances analysis of noradrenaline, adrenaline, dipivefrine, ephedrine and pseudoephedrine monographed in the European Pharmacopoeia 6. Copyright 2010 Elsevier B.V. All rights reserved.

Development and validation of a fast static headspace GC method for determination of residual solvents in permethrin.

PubMed

Tian, Jingzhi; Rustum, Abu

2016-09-05

A fast static headspace gas chromatography (HS-GC) method was developed to separate all residual solvents present in commercial active pharmaceutical ingredient (API) batches of permethrin. A total of six residual solvents namely 2-methylpentane, 3-methylpentane, methylcyclopentane, n-hexane, cyclohexane and toluene were found in typical commercial batches of permethrin; and three of them are not in the list of ICH solvents. All six residual solvents were baseline separated in five minutes by the new method presented in this paper. The method was successfully validated as per International Conference on Harmonisation (ICH) guidelines. Evaluation of this method was conducted to separate 26 commonly used solvents in the manufacturing of various APIs, key intermediates of APIs and pharmaceutical excipients. The results of the evaluation demonstrated that this method can also be used as a general method to determine residual solvents in various APIs, intermediates and excipients that are used in pharmaceutical products. Copyright © 2016 Elsevier B.V. All rights reserved.

An improved UHPLC-UV method for separation and quantification of carotenoids in vegetable crops.

PubMed

Maurer, Megan M; Mein, Jonathan R; Chaudhuri, Swapan K; Constant, Howard L

2014-12-15

Carotenoid identification and quantitation is critical for the development of improved nutrition plant varieties. Industrial analysis of carotenoids is typically carried out on multiple crops with potentially thousands of samples per crop, placing critical needs on speed and broad utility of the analytical methods. Current chromatographic methods for carotenoid analysis have had limited industrial application due to their low throughput, requiring up to 60 min for complete separation of all compounds. We have developed an improved UHPLC-UV method that resolves all major carotenoids found in broccoli (Brassica oleracea L. var. italica), carrot (Daucus carota), corn (Zea mays), and tomato (Solanum lycopersicum). The chromatographic method is completed in 13.5 min allowing for the resolution of the 11 carotenoids of interest, including the structural isomers lutein/zeaxanthin and α-/β-carotene. Additional minor carotenoids have also been separated and identified with this method, demonstrating the utility of this method across major commercial food crops. Copyright © 2014 Elsevier Ltd. All rights reserved.

Exosome separation using microfluidic systems: size-based, immunoaffinity-based and dynamic methodologies.

PubMed

Yang, Fang; Liao, Xiangzhi; Tian, Yuan; Li, Guiying

2017-04-01

Exosomes, nanovesicles secreted by most types of cells, exist in virtually all bodily fluids. Their rich nucleic acid and protein content make them potentially valuable biomarkers for noninvasive molecular diagnostics. They also show promise, after further development, to serve as a drug delivery system. Unfortunately, existing exosome separation technologies, such as ultracentrifugation and methods incorporating magnetic beads, are time-consuming, laborious and separate only exosomes of low purity. Thus, a more effective separation method is highly desirable. Microfluidic platforms are ideal tools for exosome separation, since they enable fast, cost-efficient, portable and precise processing of nanoparticles and small volumes of liquid samples. Recently, several microfluidic-based exosome separation technologies have been studied. In this article, the advantages of the most recent technologies, as well as their limitations, challenges and potential uses in novel microfluidic exosome separation and collection applications is reviewed. This review outlines the uses of new powerful microfluidic exosome detection tools for biologists and clinicians, as well as exosome separation tools for microfluidic engineers. Current challenges of exosome separation methodologies are also described, in order to highlight areas for future research and development. Copyright © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Crash prediction method for freeway facilities with high occupancy vehicle (HOV) and high occupancy toll (HOT) lanes.

DOT National Transportation Integrated Search

2015-07-01

This study developed methods for estimating the expected crash frequency of urban freeway segments : with HOV or HOT lanes. The safety impacts of the type of separation between the managed lanes and : general purpose lanes were examined. Separate mod...

Justification of rapid prototyping in the development cycle of thermoplastic-based lab-on-a-chip.

PubMed

Preywisch, Regina; Ritzi-Lehnert, Marion; Drese, Klaus S; Röser, Tina

2011-11-01

During the developmental cycle of lab-on-a-chip devices, various microstructuring techniques are required. While in the designing and assay implementation phase direct structuring or so-called rapid-prototyping methods such as milling or laser ablation are applied, replication methods like hot embossing or injection moulding are favourable for large quantity manufacturing. This work investigated the applicability of rapid-prototyping techniques for thermoplastic chip development in general, and the reproducibility of performances in dependency of the structuring technique. A previously published chip for prenatal diagnosis that preconcentrates DNA via electrokinetic trapping and field-amplified-sample-stacking and afterwards separates it in CGE was chosen as a model. The impact of structuring, sealing, and the integration of membranes on the mobility of the EOF, DNA preconcentration, and DNA separation was studied. Structuring methods were found to significantly change the location where preconcentration of DNA occurs. However, effects on the mobility of the EOF and the separation quality of DNA were not observed. Exchange of the membrane has no effect on the chip performance, whereas the sealing method impairs the separation of DNA within the chip. The overall assay performance is not significantly influenced by different structuring methods; thus, the application of rapid-prototyping methods during a chip development cycle is well justified. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Development of a process for separation of mogroside V from Siraitia grosvenorii by macroporous resins.

PubMed

Zhang, Min; Yang, Huihua; Zhang, Hongyang; Wang, Yuerong; Hu, Ping

2011-08-25

A separation method was developed for the preparative separation and enrichment of the non-caloric sweetener mogroside V from Siraitia grosvenorii. The adsorption properties of six macroporous resins were evaluated. Results showed that HZ 806 resin offered the best adsorption and desorption capacities. Based on the adsorption experiments on HZ 806, the adsorption data were found to fit the Freundlich model well. The pseudo-second-order kinetic model showed the highest correlation with the experimental results. Separation was performed with deionized water and 40% aqueous ethanol solution as mobile phases. In a typical run, 100 g of herb was processed and 3.38 g of mogroside V with a purity of 10.7% was harvested. This separation method provided a 15.1-fold increase in the purification factor from 0.5% to 10.7%. The present study showed that HZ 806 resins were effective for the separation and enrichment of mogroside V from S. grosvenorii.

A study of commuter airplane design optimization

NASA Technical Reports Server (NTRS)

Keppel, B. V.; Eysink, H.; Hammer, J.; Hawley, K.; Meredith, P.; Roskam, J.

1978-01-01

The usability of the general aviation synthesis program (GASP) was enhanced by the development of separate computer subroutines which can be added as a package to this assembly of computerized design methods or used as a separate subroutine program to compute the dynamic longitudinal, lateral-directional stability characteristics for a given airplane. Currently available analysis methods were evaluated to ascertain those most appropriate for the design functions which the GASP computerized design program performs. Methods for providing proper constraint and/or analysis functions for GASP were developed as well as the appropriate subroutines.

SEPARATED FLOW CONDITIONS AT PIPE WALLS OF WATER DISTRIBUTION MAINS - Project Summary

EPA Science Inventory

The objectives of this research project were to develop and evaluate a method for determining residence times for separated recirculation cavity flow conditions, and to determine the rate of growth and surface ramp contours developed from particulate deposits at obstacles that i...

Determination of lithium in rocks: Fluorometric method

USGS Publications Warehouse

White, C.E.; Fletcher, M.H.; Parks, J.

1951-01-01

The gravimetric method in general use for the determination of lithium is tedious, and the final weighed product often contains other alkali metals. A fluorometric method was developed to shorten the time required for the analysis and to assure that the final determination is for lithium alone. This procedure is based on the complex formed between lithium and 8-hydroxyquinoline. The fluorescence is developed in a slightly alkaline solution of 95% alcohol and measurement is made on a photoelectric fluorometer. Separation from the ore is carried out by the wet method or by the distillation procedure. Sodium and potassium are removed by alcohol and ether, but complete separation is not necessary. Comparison of analyzed samples shows excellent agreement with spectrographic and gravimetric methods. The fluorometric method is more rapid than the gravimetric and produces more conclusive results. Another useful application is in the preparation of standard lithium solutions from reagent quality salts when a known standard is available. In this case no separations are necessary.

Immobilized monolithic enzymatic reactor and its application for analysis of in-vitro fertilization media samples.

PubMed

Chen, Wei-Qiang; Obermayr, Philipp; Černigoj, Urh; Vidič, Jana; Panić-Janković, Tanta; Mitulović, Goran

2017-11-01

Classical proteomics approaches involve enzymatic hydrolysis of proteins (either separated by polyacrylamide gels or in solution) followed by peptide identification using LC-MS/MS analysis. This method requires normally more than 16 h to complete. In the case of clinical analysis, it is of the utmost importance to provide fast and reproducible analysis with minimal manual sample handling. Herein we report the method development for online protein digestion on immobilized monolithic enzymatic reactors (IMER) to accelerate protein digestion, reduce manual sample handling, and provide reproducibility to the digestion process in clinical laboratory. An integrated online digestion and separation method using monolithic immobilized enzymatic reactor was developed and applied to digestion and separation of in-vitro-fertilization media. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

[Development of an automatic vacuum liquid chromatographic device and its application in the separation of the components from Schisandra chinensis (Turz) Baill].

PubMed

Zhu, Jingbo; Liu, Baoyue; Shan, Shibo; Ding, Yanl; Kou, Zinong; Xiao, Wei

2015-08-01

In order to meet the needs of efficient purification of products from natural resources, this paper developed an automatic vacuum liquid chromatographic device (AUTO-VLC) and applied it to the component separation of petroleum ether extracts of Schisandra chinensis (Turcz) Baill. The device was comprised of a solvent system, a 10-position distribution valve, a 3-position changes valve, dynamic axis compress chromatographic columns with three diameters, and a 10-position fraction valve. The programmable logic controller (PLC) S7- 200 was adopted to realize the automatic control and monitoring of the mobile phase changing, column selection, separation time setting and fraction collection. The separation results showed that six fractions (S1-S6) of different chemical components from 100 g Schisandra chinensis (Turcz) Baill. petroleum ether phase were obtained by the AUTO-VLC with 150 mm diameter dynamic axis compress chromatographic column. A new method used for the VLC separation parameters screened by using multiple development TLC was developed and confirmed. The initial mobile phase of AUTO-VLC was selected by taking Rf of all the target compounds ranging from 0 to 0.45 for fist development on the TLC; gradient elution ratio was selected according to k value (the slope of the linear function of Rf value and development times on the TLC) and the resolution of target compounds; elution times (n) were calculated by the formula n ≈ ΔRf/k. A total of four compounds with the purity more than 85% and 13 other components were separated from S5 under the selected conditions for only 17 h. Therefore, the development of the automatic VLC and its method are significant to the automatic and systematic separation of traditional Chinese medicines.

Separation, isolation and stereochemical assignment of imazalil enantiomers and their quantitation in an in vitro toxicity test.

PubMed

Casas, Mònica Escolà; Kretschmann, Andreas Christopher; Andernach, Lars; Opatz, Till; Bester, Kai

2016-06-24

A simple method for the separation of the enantiomers of the fungicide imazalil was developed. Racemic imazalil was separated into its enantiomers with an enantiomeric purity of 99% using HPLC-UV with an enantioselective column (permethylated cyclodextrin) operated in reversed phase mode (water with 0.2% trimethylamine and 0.08% acetic acid and methanol). The absolute configuration of the separated enantiomers was assigned and unequivocally confirmed by optical rotation as well as by vibrational circular dichroism (VCD) and electronic circular dichroism (ECD) combined with ab-initio calculations. The same enantioselective column was also used to develop an HPLC-MS/MS method for the quantification of imazalil enantiomers. The HPLC-MS/MS method reached limits of quantification (LOQs) of 0.025mg/mL with 5μL injections. This method was used to verify imazalil concentrations and enantiomeric fractions in samples from an in vitro test on effects on human steroidogenesis (H295R steroidogenesis assay). The quantification verified the stability of the enantiomers of imazalil during the in vitro tests. Copyright © 2016 Elsevier B.V. All rights reserved.

Modern Approach to Medical Diagnostics - the Use of Separation Techniques in Microorganisms Detection.

PubMed

Chylewska, Agnieszka; Ogryzek, M; Makowski, Mariusz

2017-10-23

New analytical and molecular methods for microorganisms are being developed on various features of identification i.e. selectivity, specificity, sensitivity, rapidity and discrimination of the viable cell. The presented review was established following the current trends in improved pathogens separation and detection methods and their subsequent use in medical diagnosis. This contribution also focuses on the development of analytical and biological methods in the analysis of microorganisms, with special attention paid to bio-samples containing microbes (blood, urine, lymph, wastewater). First, the paper discusses microbes characterization, their structure, surface, properties, size and then it describes pivotal points in the bacteria, viruses and fungi separation procedure obtained by researchers in the last 30 years. According to the above, detection techniques can be classified into three categories, which were, in our opinion, examined and modified most intensively during this period: electrophoretic, nucleic-acid-based, and immunological methods. The review covers also the progress, limitations and challenges of these approaches and emphasizes the advantages of new separative techniques in selective fractionating of microorganisms. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

Linear solvation energy relationships in normal phase chromatography based on gradient separations.

PubMed

Wu, Di; Lucy, Charles A

2017-09-22

Coupling the modified Soczewiñski model and one gradient run, a gradient method was developed to build a linear solvation energy relationship (LSER) for normal phase chromatography. The gradient method was tested on dinitroanilinopropyl (DNAP) and silica columns with hexane/dichloromethane (DCM) mobile phases. LSER models built based on the gradient separation agree with those derived from a series of isocratic separations. Both models have similar LSER coefficients and comparable goodness of fit, but the LSER model based on gradient separation required fewer trial and error experiments. Copyright © 2017 Elsevier B.V. All rights reserved.

A Methodology for Anatomic Ultrasound Image Diagnostic Quality Assessment.

PubMed

Hemmsen, Martin Christian; Lange, Theis; Brandt, Andreas Hjelm; Nielsen, Michael Bachmann; Jensen, Jorgen Arendt

2017-01-01

This paper discusses the methods for the assessment of ultrasound image quality based on our experiences with evaluating new methods for anatomic imaging. It presents a methodology to ensure a fair assessment between competing imaging methods using clinically relevant evaluations. The methodology is valuable in the continuing process of method optimization and guided development of new imaging methods. It includes a three phased study plan covering from initial prototype development to clinical assessment. Recommendations to the clinical assessment protocol, software, and statistical analysis are presented. Earlier uses of the methodology has shown that it ensures validity of the assessment, as it separates the influences between developer, investigator, and assessor once a research protocol has been established. This separation reduces confounding influences on the result from the developer to properly reveal the clinical value. This paper exemplifies the methodology using recent studies of synthetic aperture sequential beamforming tissue harmonic imaging.

Separation of porphyrin-based photosensitizer isomers by laser-induced fluorescence capillary electrophoresis.

PubMed

Peng, Xuejun; Sternberg, Ethan; Dolphin, David

2005-10-01

Methods for the separation of photosensitizer isomers, such as benzoporphyrin derivative monoacid, benzoporphyrin ethyl monoacid, 2-[1-hexyloxyethyl]-2-devinylpyropheophorbide-a, diethyleneglycol diester benzoporphyrin derivative, tin ethyl etiopurpurin, and phthalocyanine tetrasulfonate, have been systematically developed by CE. Detection was accomplished by UV absorption at 214 nm or by LIF with excitation at 442/488 nm and emission at 690 nm. The effects of three major experimental parameters of buffer types, organic solvents, and surfactant additives are described. The optimized separation conditions were determined so as to provide satisfactory separation efficiency and analysis time. The methods are shown to be suitable for the separation and determination of porphyrin and phthalocyanines regioisomers, diastereoisomers, and enantiomers.

Seismoelectric data processing for surface surveys of shallow targets

USGS Publications Warehouse

Haines, S.S.; Guitton, A.; Biondi, B.

2007-01-01

The utility of the seismoelectric method relies on the development of methods to extract the signal of interest from background and source-generated coherent noise that may be several orders-of-magnitude stronger. We compare data processing approaches to develop a sequence of preprocessing and signal/noise separation and to quantify the noise level from which we can extract signal events. Our preferred sequence begins with the removal of power line harmonic noise and the use of frequency filters to minimize random and source-generated noise. Mapping to the linear Radon domain with an inverse process incorporating a sparseness constraint provides good separation of signal from noise, though it is ineffective on noise that shows the same dip as the signal. Similarly, the seismoelectric signal and noise do not separate cleanly in the Fourier domain, so f-k filtering can not remove all of the source-generated noise and it also disrupts signal amplitude patterns. We find that prediction-error filters provide the most effective method to separate signal and noise, while also preserving amplitude information, assuming that adequate pattern models can be determined for the signal and noise. These Radon-domain and prediction-error-filter methods successfully separate signal from <33 dB stronger noise in our test data. ?? 2007 Society of Exploration Geophysicists.

Bacteriophage-based nanoprobes for rapid bacteria separation

NASA Astrophysics Data System (ADS)

Chen, Juhong; Duncan, Bradley; Wang, Ziyuan; Wang, Li-Sheng; Rotello, Vincent M.; Nugen, Sam R.

2015-10-01

The lack of practical methods for bacterial separation remains a hindrance for the low-cost and successful development of rapid detection methods from complex samples. Antibody-tagged magnetic particles are commonly used to pull analytes from a liquid sample. While this method is well-established, improvements in capture efficiencies would result in an increase of the overall detection assay performance. Bacteriophages represent a low-cost and more consistent biorecognition element as compared to antibodies. We have developed nanoscale bacteriophage-tagged magnetic probes, where T7 bacteriophages were bound to magnetic nanoparticles. The nanoprobe allowed the specific recognition and attachment to E. coli cells. The phage magnetic nanprobes were directly compared to antibody-conjugated magnetic nanoprobes. The capture efficiencies of bacteriophages and antibodies on nanoparticles for the separation of E. coli K12 at varying concentrations were determined. The results indicated a similar bacteria capture efficiency between the two nanoprobes.The lack of practical methods for bacterial separation remains a hindrance for the low-cost and successful development of rapid detection methods from complex samples. Antibody-tagged magnetic particles are commonly used to pull analytes from a liquid sample. While this method is well-established, improvements in capture efficiencies would result in an increase of the overall detection assay performance. Bacteriophages represent a low-cost and more consistent biorecognition element as compared to antibodies. We have developed nanoscale bacteriophage-tagged magnetic probes, where T7 bacteriophages were bound to magnetic nanoparticles. The nanoprobe allowed the specific recognition and attachment to E. coli cells. The phage magnetic nanprobes were directly compared to antibody-conjugated magnetic nanoprobes. The capture efficiencies of bacteriophages and antibodies on nanoparticles for the separation of E. coli K12 at varying concentrations were determined. The results indicated a similar bacteria capture efficiency between the two nanoprobes. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr03779d

Environmental and human monitoring of Americium-241 utilizing extraction chromatography and alpha-spectrometry.

PubMed

Goldstein, S J; Hensley, C A; Armenta, C E; Peters, R J

1997-03-01

Recent developments in extraction chromatography have simplified the separation of americium from complex matrices in preparation for alpha-spectroscopy relative to traditional methods. Here we present results of procedures developed/adapted for water, air, and bioassay samples with less than 1 g of inorganic residue. Prior analytical methods required the use of a complex, multistage procedure for separation of americium from these matrices. The newer, simplified procedure requires only a single 2 mL extraction chromatographic separation for isolation of Am and lanthanides from other components of the sample. This method has been implemented on an extensive variety of "real" environmental and bioassay samples from the Los Alamos area, and consistently reliable and accurate results with appropriate detection limits have been obtained. The new method increases analytical throughput by a factor of approximately 2 and decreases environmental hazards from acid and mixed-waste generation relative to the prior technique. Analytical accuracy, reproducibility, and reliability are also significantly improved over the more complex and laborious method used previously.

Computation of subsonic flow around airfoil systems with multiple separation

NASA Technical Reports Server (NTRS)

Jacob, K.

1982-01-01

A numerical method for computing the subsonic flow around multi-element airfoil systems was developed, allowing for flow separation at one or more elements. Besides multiple rear separation also sort bubbles on the upper surface and cove bubbles can approximately be taken into account. Also, compressibility effects for pure subsonic flow are approximately accounted for. After presentation the method is applied to several examples and improved in some details. Finally, the present limitations and desirable extensions are discussed.

Foam separation of Rhodamine-G and Evans Blue using a simple separatory bottle system.

PubMed

Dasarathy, Dhweeja; Ito, Yoichiro

2017-09-29

A simple separatory glass bottle was used to improve separation effectiveness and cost efficiency while simultaneously creating a simpler system for separating biological compounds. Additionally, it was important to develop a scalable separation method so this would be applicable to both analytical and preparative separations. Compared to conventional foam separation methods, this method easily forms stable dry foam which ensures high purity of yielded fractions. A negatively charged surfactant, sodium dodecyl sulfate (SDS), was used as the ligand to carry a positively charged Rhodamine-G, leaving a negatively charged Evans Blue in the bottle. The performance of the separatory bottle was tested for separating Rhodamine-G from Evans Blue with sample sizes ranged from 1 to 12mg in preparative separations and 1-20μg in analytical separations under optimum conditions. These conditions including N 2 gas pressure, spinning speed of contents with a magnetic stirrer, concentration of the ligand, volume of the solvent, and concentration of the sample, were all modified and optimized. Based on the calculations at their peak absorbances, Rhodamine-G and Evans Blue were efficiently separated in times ranging from 1h to 3h, depending on sample volume. Optimal conditions were found to be 60psi N 2 pressure and 2mM SDS for the affinity ligand. This novel separation method will allow for rapid separation of biological compounds while simultaneously being scalable and cost effective. Published by Elsevier B.V.

Quantitative separation of tetralin hydroperoxide from its decomposition products by high performance liquid chromatography

NASA Technical Reports Server (NTRS)

Worstell, J. H.; Daniel, S. R.

1981-01-01

A method for the separation and analysis of tetralin hydroperoxide and its decomposition products by high pressure liquid chromatography has been developed. Elution with a single, mixed solvent from a micron-Porasil column was employed. Constant response factors (internal standard method) over large concentration ranges and reproducible retention parameters are reported.

Enhancing resolution of free-flow zone electrophoresis via a simple sheath-flow sample injection.

PubMed

Yang, Ying; Kong, Fan-Zhi; Liu, Ji; Li, Jun-Min; Liu, Xiao-Ping; Li, Guo-Qing; Wang, Ju-Fang; Xiao, Hua; Fan, Liu-Yin; Cao, Cheng-Xi; Li, Shan

2016-07-01

In this work, a simple and novel sheath-flow sample injection method (SFSIM) is introduced to reduce the band broadening of free-flow zone electrophoresis separation in newly developed self-balance free-flow electrophoresis instrument. A needle injector was placed in the center of the separation inlet, into which the BGE and sample solution were pumped simultaneously. BGE formed sheath flow outside the sample stream, resulting in less band broadening related to hydrodynamics and electrodynamics. Hemoglobin and C-phycocyanin were successfully separated by the proposed method in contrast to the poor separation of free-flow electrophoresis with the traditional injection method without sheath flow. About 3.75 times resolution enhancement could be achieved by sheath-flow sample injection method. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A new open tubular capillary microextraction and sweeping for the analysis of super low concentration of hydrophobic compounds.

PubMed

Xia, Zhining; Gan, Tingting; Chen, Hua; Lv, Rui; Wei, Weili; Yang, Fengqing

2010-10-01

A sample pre-concentration method based on the in-line coupling of in-tube solid-phase microextraction and electrophoretic sweeping was developed for the analysis of hydrophobic compounds. The sample pre-concentration and electrophoretic separation processes were simply and sequentially carried out with a (35%-phenyl)-methylpolysiloxane-coated capillary. The developed method was validated and applied to enrich and separate several pharmaceuticals including loratadine, indomethacin, ibuprofen and doxazosin. Several parameters of microextration were investigated such as temperature, pH and eluant. And the concentration of microemulsion that influences separation efficiency and microextraction efficiency were also studied. Central composite design was applied for the optimization of sampling flow rate and sampling time that interact in a very complex way with each other. The precision, sensitivity and recovery of the method were investigated. Under the optimal conditions, the maximum enrichment factors for loratadine, indomethacin, ibuprofen and doxazosin in aqueous solutions are 1355, 571, 523 and 318, respectively. In addition, the developed method was applied to determine loratadine in rabbit blood sample.

Initial evaluation of a convection counter streaming galvanization technique of sex separation of human spermatozoa.

PubMed

Daniell, J F; Herbert, C M; Repp, J; Torbit, C A; Wentz, A C

1982-08-01

A new method for separating X and Y human spermatozoa called convection counter streaming galvanization was evaluated. The method was independently performed by this semenology laboratory with the use of the special separation equipment and extending media provided by its developer, Dr. Bhairab C. Bhattacharya. The mean number of Y spermatozoa increased from 48% to 77% in the separated fraction predicted to be Y-enriched. The fraction predicted to be X-enriched increased from a mean of 52% to 77%. The one separation process allowed accumulation of both enriched fractions simultaneously. The separated portions of spermatozoa maintained good motility and penetration of cervical mucus but produced a mean recovery concentration in the X- and Y-enriched fractions of only 15% to 16% of the preseparation concentration.

Preliminary Tests For Development Of A Non-Pertechnetate Analysis Method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Diprete, D.; McCabe, D.

2016-09-28

The objective of this task was to develop a non-pertechnetate analysis method that 222-S lab could easily implement. The initial scope involved working with 222-S laboratory personnel to adapt the existing Tc analytical method to fractionate the non-pertechnetate and pertechnetate. SRNL then developed and tested a method using commercial sorbents containing Aliquat ® 336 to extract the pertechnetate (thereby separating it from non-pertechnetate), followed by oxidation, extraction, and stripping steps, and finally analysis by beta counting and Mass Spectroscopy. Several additional items were partially investigated, including impacts of a 137Cs removal step. The method was initially tested on SRS tankmore » waste samples to determine its viability. Although SRS tank waste does not contain non-pertechnetate, testing with it was useful to investigate the compatibility, separation efficiency, interference removal efficacy, and method sensitivity.« less

DryLab® optimised two-dimensional high performance liquid chromatography for differentiation of ephedrine and pseudoephedrine based methamphetamine samples.

PubMed

Andrighetto, Luke M; Stevenson, Paul G; Pearson, James R; Henderson, Luke C; Conlan, Xavier A

2014-11-01

In-silico optimised two-dimensional high performance liquid chromatographic (2D-HPLC) separations of a model methamphetamine seizure sample are described, where an excellent match between simulated and real separations was observed. Targeted separation of model compounds was completed with significantly reduced method development time. This separation was completed in the heart-cutting mode of 2D-HPLC where C18 columns were used in both dimensions taking advantage of the selectivity difference of methanol and acetonitrile as the mobile phases. This method development protocol is most significant when optimising the separation of chemically similar chemical compounds as it eliminates potentially hours of trial and error injections to identify the optimised experimental conditions. After only four screening injections the gradient profile for both 2D-HPLC dimensions could be optimised via simulations, ensuring the baseline resolution of diastereomers (ephedrine and pseudoephedrine) in 9.7 min. Depending on which diastereomer is present the potential synthetic pathway can be categorized.

Separation and sorting of cells in microsystems using physical principles

NASA Astrophysics Data System (ADS)

Lee, Gi-Hun; Kim, Sung-Hwan; Ahn, Kihoon; Lee, Sang-Hoon; Park, Joong Yull

2016-01-01

In the last decade, microfabrication techniques have been combined with microfluidics and applied to cell biology. Utilizing such new techniques, various cell studies have been performed for the research of stem cells, immune cells, cancer, neurons, etc. Among the various biological applications of microtechnology-based platforms, cell separation technology has been highly regarded in biological and clinical fields for sorting different types of cells, finding circulating tumor cells (CTCs), and blood cell separation, amongst other things. Many cell separation methods have been created using various physical principles. Representatively, these include hydrodynamic, acoustic, dielectrophoretic, magnetic, optical, and filtering methods. In this review, each of these methods will be introduced, and their physical principles and sample applications described. Each physical principle has its own advantages and disadvantages. The engineers who design the systems and the biologists who use them should understand the pros and cons of each method or principle, to broaden the use of microsystems for cell separation. Continuous development of microsystems for cell separation will lead to new opportunities for diagnosing CTCs and cancer metastasis, as well as other elements in the bloodstream.

Development of micropump-actuated negative pressure pinched injection for parallel electrophoresis on array microfluidic chip.

PubMed

Li, Bowei; Jiang, Lei; Xie, Hua; Gao, Yan; Qin, Jianhua; Lin, Bingcheng

2009-09-01

A micropump-actuated negative pressure pinched injection method is developed for parallel electrophoresis on a multi-channel LIF detection system. The system has a home-made device that could individually control 16-port solenoid valves and a high-voltage power supply. The laser beam is excitated and distributes to the array separation channels for detection. The hybrid Glass-PDMS microfluidic chip comprises two common reservoirs, four separation channels coupled to their respective pneumatic micropumps and two reference channels. Due to use of pressure as a driving force, the proposed method has no sample bias effect for separation. There is only one high-voltage supply needed for separation without relying on the number of channels, which is significant for high-throughput analysis, and the time for sample loading is shortened to 1 s. In addition, the integrated micropumps can provide the versatile interface for coupling with other function units to satisfy the complicated demands. The performance is verified by separation of DNA marker and Hepatitis B virus DNA samples. And this method is also expected to show the potential throughput for the DNA analysis in the field of disease diagnosis.

Supercritical fluids in separation science--the dreams, the reality and the future.

PubMed

Smith, R M

1999-09-24

The last 20 years have seen an intense interest in the use of supercritical fluids in separation science. This started with the introduction of commercial instruments first for packed and then for capillary chromatography and it looked as if this would be a technique to rival gas-liquid chromatography and HPLC. The activity developed quite rapidly into packed column supercritical fluid separations then into supercritical fluid extraction. However, in recent years there has been a decline in publications. These later techniques continue to be used but are now principally applied to a limited group of applications where they offer significant advantages over alternative techniques. This review looks back over this period and analyses how these methods were developed and the fluids, detectors and applications that were examined. It suggests why many of the initial applications have vanished and why the initial apparent promise was not fulfilled. The rise and fall of supercritical fluids represents a lesson in the way analysts approach new techniques and how we might view other new separation developments at the end of this millennium. The review looks forward to the future of supercritical fluids and their role at the end of the first century of separation science. Probably the most important idea that supercritical fluids have brought to separation science is a recognition that there is unity in the separation methods and that a continuum exists from gases to liquids.

Development and validation of an analytical method for the separation and determination of major bioactive curcuminoids in Curcuma longa rhizomes and herbal products using non-aqueous capillary electrophoresis.

PubMed

Anubala, S; Sekar, R; Nagaiah, K

2014-06-01

A simple, fast and efficient non-aqueous capillary electrophoresis method (NACE) was developed for the simultaneous determination of three major bioactive curcuminoids (CMNs) in Curcuma longa rhizomes and its herbal products. Good separation, resolution and reproducibility were achieved with the background electrolyte (BGE) consisting a mixture of 15.0 mM sodium tetraborate and 7.4 mM sodium hydroxide (NaOH) in 2:10:15 (v/v/v) of water, 1-propanol, and methanol. The influences of background electrolyte, sodium hydroxide, water, sodium dodecyl sulfate and hydroxylpropyl-β-cyclodextrin on separations were investigated. The separation was carried out in a fused-silica capillary tube with reverse polarity. Hydrodynamic injection of 25mbar for 12s was used for injecting samples and a voltage of 28 kV was applied for separation. The ultrasonication method was used for the extraction of CMNs from the turmeric herbal products and the extract was filtered and directly injected without any further treatments. The limits of detection and quantification were less than 5.0 and 14.6 µg/ml respectively for all CMNs. The percentage recoveries for CMNs were >97.2% (%RSD, <2.62). The results obtained by the method were compared with existing spectrophotometric and HPLC methods. The related compounds in the extract did not interfere in the determination of CMNs. The proposed NACE method is better than existing chromatographic and electrophoretic methods in terms of simple electrophoretic medium, fast analysis and good resolution. Copyright © 2014 Elsevier B.V. All rights reserved.

A validated stability-indicating LC method for the separation of enantiomer and potential impurities of Linezolid using polar organic mode.

PubMed

Satyanarayana Raju, T; Vishweshwari Kutty, O; Ganesh, V; Yadagiri Swamy, P

2012-08-01

Although a number of methods are available for evaluating Linezolid and its possible impurities, a common method for separation if its potential impurities, degradants and enantiomer in a single method with good efficiency remain unavailable. With the objective of developing an advanced method with shorter runtimes, a simple, precise, accurate stability-indicating LC method was developed for the determination of purity of Linezolid drug substance and drug products in bulk samples and pharmaceutical dosage forms in the presence of its impurities and degradation products. This method is capable of separating all the related substances of Linezolid along with the chiral impurity. This method can also be used for the estimation of assay of Linezolid in drug substance as well as in drug product. The method was developed using Chiralpak IA (250 mm×4.6 mm, 5 μm) column. A mixture of acetonitrile, ethanol, n-butyl amine and trifluoro acetic acid in 96:4:0.10:0.16 (v/v/v/v) ratio was used as a mobile phase. The eluted compounds were monitored at 254 nm. Linezolid was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal and photolytic degradation. The degradation products were well resolved from main peak and its impurities, proving the stability-indicating power of the method. The developed method was validated as per International Conference on Harmonization (ICH) guidelines with respect to specificity, limit of detection, limit of quantification, precision, linearity, accuracy, robustness and system suitability.

UHPLC-UV method for the determination of flavonoids in dietary supplements and for evaluation of their antioxidant activities.

PubMed

Magiera, Sylwia; Baranowska, Irena; Lautenszleger, Anna

2015-01-01

A simple and rapid ultra-high performance liquid chromatographic (UHPLC) method coupled with an ultraviolet detector (UV) has been developed and validated for the separation and determination of 14 major flavonoids ((±)-catechin, (-)-epicatechin, glycitin, (-)-epicatechin gallate, rutin, quercitrin, hesperidine, neohesperidine, daidzein, glycitein, quercetin, genistein, hesperetin, and biochanin A) in herbal dietary supplements. The flavonoids have been separated on a Chromolith Fast Gradient Monolithic RP-18e column utilizing a mobile phase composed of 0.05% trifluoroacetic acid in water and acetonitrile in gradient elution mode. Under these conditions, flavonoids were separated in a 5 min run. The selectivity of the developed UHPLC-UV method was confirmed by comparison with ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) analysis. The validation parameters such as linearity, sensitivity, precision, and accuracy were found to be highly satisfactory. The optimized method was applied to determination of flavonoids in different dietary supplements. Additionally, the developed HPLC-UV method combined with 2,2-diphenyl-1-picrylhydrazyl radical (DPPH) assay was used in the evaluation of antioxidant activity of the selected flavonoids. Copyright © 2014 Elsevier B.V. All rights reserved.

Homogeneous Immunoassays: Historical Perspective and Future Promise

NASA Astrophysics Data System (ADS)

Ullman, Edwin F.

1999-06-01

The founding and growth of Syva Company is examined in the context of its leadership role in the development of homogeneous immunoassays. The simple mix and read protocols of these methods offer advantages in routine analytical and clinical applications. Early homogeneous methods were based on insensitive detection of immunoprecipitation during antigen/antibody binding. The advent of reporter groups in biology provided a means of quantitating immunochemical binding by labeling antibody or antigen and physically separating label incorporated into immune complexes from free label. Although high sensitivity was achieved, quantitative separations were experimentally demanding. Only when it became apparent that reporter groups could provide information, not only about the location of a molecule but also about its microscopic environment, was it possible to design practical non-separation methods. The evolution of early homogenous immunoassays was driven largely by the development of improved detection strategies. The first commercial spin immunoassays, developed by Syva for drug abuse testing during the Vietnam war, were followed by increasingly powerful methods such as immunochemical modulation of enzyme activity, fluorescence, and photo-induced chemiluminescence. Homogeneous methods that quantify analytes at femtomolar concentrations within a few minutes now offer important new opportunities in clinical diagnostics, nucleic acid detection and drug discovery.

RAPID METHOD FOR DETERMINATION OF RADIOSTRONTIUM IN EMERGENCY MILK SAMPLES

DOE Office of Scientific and Technical Information (OSTI.GOV)

Maxwell, S.; Culligan, B.

2008-07-17

A new rapid separation method for radiostrontium in emergency milk samples was developed at the Savannah River Site (SRS) Environmental Bioassay Laboratory (Aiken, SC, USA) that will allow rapid separation and measurement of Sr-90 within 8 hours. The new method uses calcium phosphate precipitation, nitric acid dissolution of the precipitate to coagulate residual fat/proteins and a rapid strontium separation using Sr Resin (Eichrom Technologies, Darien, IL, USA) with vacuum-assisted flow rates. The method is much faster than previous method that use calcination or cation exchange pretreatment, has excellent chemical recovery, and effectively removes beta interferences. When a 100 ml samplemore » aliquot is used, the method has a detection limit of 0.5 Bq/L, well below generic emergency action levels.« less

Continuous flow microfluidic separation and processing of rare cells and bioparticles found in blood - A review.

PubMed

Antfolk, Maria; Laurell, Thomas

2017-05-01

Rare cells in blood, such as circulating tumor cells or fetal cells in the maternal circulation, posses a great prognostic or diagnostic value, or for the development of personalized medicine, where the study of rare cells could provide information to more specifically targeted treatments. When conventional cell separation methods, such as flow cytometry or magnetic activated cell sorting, have fallen short other methods are desperately sought for. Microfluidics have been extensively used towards isolating and processing rare cells as it offers possibilities not present in the conventional systems. Furthermore, microfluidic methods offer new possibilities for cell separation as they often rely on non-traditional biomarkers and intrinsic cell properties. This offers the possibility to isolate cell populations that would otherwise not be targeted using conventional methods. Here, we provide an extensive review of the latest advances in continuous flow microfluidic rare cell separation and processing with each cell's specific characteristics and separation challenges as a point of view. Copyright © 2017 Elsevier B.V. All rights reserved.

Rapid determination of thermodynamic parameters from one-dimensional programmed-temperature gas chromatography for use in retention time prediction in comprehensive multidimensional chromatography.

PubMed

McGinitie, Teague M; Ebrahimi-Najafabadi, Heshmatollah; Harynuk, James J

2014-01-17

A new method for estimating the thermodynamic parameters of ΔH(T0), ΔS(T0), and ΔCP for use in thermodynamic modeling of GC×GC separations has been developed. The method is an alternative to the traditional isothermal separations required to fit a three-parameter thermodynamic model to retention data. Herein, a non-linear optimization technique is used to estimate the parameters from a series of temperature-programmed separations using the Nelder-Mead simplex algorithm. With this method, the time required to obtain estimates of thermodynamic parameters a series of analytes is significantly reduced. This new method allows for precise predictions of retention time with the average error being only 0.2s for 1D separations. Predictions for GC×GC separations were also in agreement with experimental measurements; having an average relative error of 0.37% for (1)tr and 2.1% for (2)tr. Copyright © 2013 Elsevier B.V. All rights reserved.

Rapid and sensitive analytical method for monitoring of 12 organotin compounds in natural waters.

PubMed

Vahčič, Mitja; Milačič, Radmila; Sčančar, Janez

2011-03-01

A rapid analytical method for the simultaneous determination of 12 different organotin compounds (OTC): methyl-, butyl-, phenyl- and octyl-tins in natural water samples was developed. It comprises of in situ derivatisation (by using NaBEt4) of OTC in salty or fresh water sample matrix adjusted to pH 6 with Tris-citrate buffer, extraction of ethylated OTC into hexane, separation of OTC in organic phase on 15 m GC column and subsequent quantitative determination of separated OTC by ICP-MS. To optimise the pH of ethylation, phosphate, carbonate and Tris-citrate buffer were investigated alternatively to commonly applied sodium acetate - acetic acid buffer. The ethylation yields in Tris-citrate buffer were found to be better for TBT, MOcT and DOcT in comparison to commonly used acetate buffer. Iso-octane and hexane were examined as organic phase for extraction of ethylated OTC. The advantage of hexane was in its ability for quantitative determination of TMeT. GC column of 15 m in length was used for separation of studied OTC under the optimised separation conditions and its performances compared to 30 m column. The analytical method developed enables sensitive simultaneous determination of 12 different OTC and appreciably shortened analysis time in larger series of water samples. LOD's obtained for the newly developed method ranged from 0.05-0.06 ng Sn L-1 for methyl-, 0.11-0.45 ng Sn L-1 for butyl-, 0.11-0.16 ng Sn L-1 for phenyl-, and 0.07-0.10 ng Sn L-1 for octyl-tins. By applying the developed analytical method, marine water samples from the Northern Adriatic Sea containing mainly butyl- and methyl-tin species were analysed to confirm the proposed method's applicability.

Simultaneous separation of water- and fat-soluble vitamins in isocratic pressure-assisted capillary electrochromatography using a methacrylate-based monolithic column.

PubMed

Yamada, Hiroki; Kitagawa, Shinya; Ohtani, Hajime

2013-06-01

A method of simultaneous separation of water- and fat-soluble vitamins using pressure-assisted CEC with a methacrylate-based capillary monolithic column was developed. In the proposed method, water-soluble vitamins were mainly separated electrophoretically, while fat soluble-ones were separated chromatographically by the interaction with a methacrylate-based monolith. A mixture of six water-soluble and four fat-soluble vitamins was separated simultaneously within 20 min with an isocratic elution using 1 M formic acid (pH 1.9)/acetonitrile (30:70, v/v) containing 10 mM ammonium formate as a mobile phase. When the method was applied to a commercial multivitamin tablet and a spiked one, the vitamins were successfully analyzed, and no influence of the matrix contained in the tablet was observed. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Analytical method development for directed enzyme evolution research: a high throughput high-performance liquid chromatography method for analysis of ribose and ribitol and a capillary electrophoresis method for the separation of ribose enantiomers.

PubMed

Sun, Baoguo; Miller, Gregory; Lee, Wan Yee; Ho, Kelvin; Crowe, Michael A; Partridge, Leslie

2013-01-04

Analytical methods were developed for a directed enzyme evolution research programme, which pursued high performance enzymes to produce high quality L-ribose using large scale biocatalytic reaction. A high throughput HPLC method with evaporative light-scattering detection was developed to test ribose and ribitol in the enzymatic reaction, a β-cyclobond 2000 analytical column separated ribose and ribitol in 2.3 min, a C(18) guard column was used as an on-line filter to clean up the enzyme sample matrix and a short gradient was applied to wash the column, the enzymatic reaction solution can be directly injected after quenching. Total run time of each sample was approx. 4 min which provided capability of screening 4×96-well plates/day/instrument. Meanwhile, a capillary electrophoresis method was developed for the separation of ribose enantiomers, while 7-aminonaphthalene-1,3-disulfonic acid was used as derivatisation reagent and 25 mM tetraborate with 5 mM β-cyclodextrin was used as electrolyte. 0.35%of D-ribose in L-ribose can be detected which can be translated into 99.3% ee of L-ribose. Derivatisation reagent and sample matrix did not interfere with the measurement. Copyright © 2012 Elsevier B.V. All rights reserved.

Separation of left and right lungs using 3D information of sequential CT images and a guided dynamic programming algorithm

PubMed Central

Park, Sang Cheol; Leader, Joseph Ken; Tan, Jun; Lee, Guee Sang; Kim, Soo Hyung; Na, In Seop; Zheng, Bin

2011-01-01

Objective this article presents a new computerized scheme that aims to accurately and robustly separate left and right lungs on CT examinations. Methods we developed and tested a method to separate the left and right lungs using sequential CT information and a guided dynamic programming algorithm using adaptively and automatically selected start point and end point with especially severe and multiple connections. Results the scheme successfully identified and separated all 827 connections on the total 4034 CT images in an independent testing dataset of CT examinations. The proposed scheme separated multiple connections regardless of their locations, and the guided dynamic programming algorithm reduced the computation time to approximately 4.6% in comparison with the traditional dynamic programming and avoided the permeation of the separation boundary into normal lung tissue. Conclusions The proposed method is able to robustly and accurately disconnect all connections between left and right lungs and the guided dynamic programming algorithm is able to remove redundant processing. PMID:21412104

Zero leakage separable and semipermanent ducting joints

NASA Technical Reports Server (NTRS)

Mischel, H. T.

1973-01-01

A study program has been conducted to explore new methods of achieving zero leakage, separable and semipermanent, ducting joints for space flight vehicles. The study consisted of a search of literature of existing zero leakage methods, the generation of concepts of new methods of achieving the desired zero leakage criteria and the development of detailed analysis and design of a selected concept. Other techniques of leak detection were explored with a view toward improving this area.

THEMIS Surface-Atmosphere Separation Strategy and Preliminary Results

NASA Technical Reports Server (NTRS)

Bandfield, J. L.; Smith, M. D.; Christensen, P. R.

2002-01-01

Methods refined and adapted from the TES investigation are used to develop a surface-atmosphere separation strategy for THEMIS image analysis and atmospheric temperature and opacity retrievals. Additional information is contained in the original extended abstract.

Separation of Membrane-Bound Compounds by Solid-Supported Bilayer Electrophoresis

PubMed Central

Daniel, Susan; Diaz, Arnaldo J.; Martinez, Kelly M.; Bench, Bennie J.; Albertorio, Fernando; Cremer, Paul S.

2008-01-01

A new method was developed to purify membrane bound species within a supported lipid bilayer (SLB) environment. SLBs consisting of phosphatidylcholine lipids and cholesterol were employed as the separation matrix. Cholesterol was used to reduce the diffusion of lipids within the bilayer and, therefore, substantially reduce mixing of the dye-conjugated lipids to be separated. These molecules were introduced into an SLB adjacent to the separations SLB and electrophoresis was employed to move these species through it. The method was powerful enough to completely resolve two isomers of Texas Red DHPE from each other. Moreover, these isomers could be separated from a BODIPY-conjugated lipid as well. Such procedures could be extended to the purification of peripheral and transmembrane proteins. PMID:17564451

Preparative separation of the polar part from the rhizomes of Anemarrhena asphodeloides using a hydrophilic C18 stationary phase.

PubMed

Cai, Jianfeng; Xin, Huaxia; Cheng, Lingping; Fu, YanHui; Jiang, Dasen; Feng, Jiatao; Fu, Qing; Jin, Yu; Liang, Xinmiao

2017-09-15

The goal of this study was to develop a method that utilized a hydrophilic C18 stationary phase in the preparative high performance liquid chromatography to isolate the polar part from the rhizomes of Anemarrhena asphodeloides. The results showed that an initial mobile phase of pure water for the separation could greatly increase the retention and solubility of the polar compounds at the preparative scale. Introducing polar groups on the surface of the hydrophilic C18 column together with the use of optimized mobile phase compositions improved the column separation selectivity for polar compounds. Eleven previously undescribed compounds in Anemarrhena asphodeloides were obtained, indicating that the method developed in this study would facilitate the purification and separation of the polar part of traditional Chinese medicines. Copyright © 2017 Elsevier B.V. All rights reserved.

Rapid determination of 210Po in water samples

DOE Office of Scientific and Technical Information (OSTI.GOV)

Maxwell, Sherrod L.; Culligan, Brian K.; Hutchison, Jay B.

2013-08-02

A new rapid method for the determination of 210Po in water samples has been developed at the Savannah River National Laboratory (SRNL) that can be used for emergency response or routine water analyses. If a radiological dispersive device (RDD) event or a radiological attack associated with drinking water supplies occurs, there will be an urgent need for rapid analyses of water samples, including drinking water, ground water and other water effluents. Current analytical methods for the assay of 210Po in water samples have typically involved spontaneous auto-deposition of 210Po onto silver or other metal disks followed by counting by alphamore » spectrometry. The auto-deposition times range from 90 minutes to 24 hours or more, at times with yields that may be less than desirable. If sample interferences are present, decreased yields and degraded alpha spectrums can occur due to unpredictable thickening in the deposited layer. Separation methods have focused on the use of Sr Resin, often in combination with 210Pb analysis. A new rapid method for 210Po in water samples has been developed at the Savannah River National Laboratory (SRNL) that utilizes a rapid calcium phosphate co-precipitation method, separation using DGA Resin (N,N,N,N-tetraoctyldiglycolamide extractant-coated resin, Eichrom Technologies or Triskem-International), followed by rapid microprecipitation of 210Po using bismuth phosphate for counting by alpha spectrometry. This new method can be performed quickly with excellent removal of interferences, high chemical yields and very good alpha peak resolution, eliminating any potential problems with the alpha source preparation for emergency or routine samples. A rapid sequential separation method to separate 210Po and actinide isotopes was also developed. This new approach, rapid separation with DGA Resin plus microprecipitation for alpha source preparation, is a significant advance in radiochemistry for the rapid determination of 210Po.« less

A modified approach for isolation of essential oil from fruit of Amorpha fruticosa Linn using microwave-assisted hydrodistillation concatenated liquid-liquid extraction.

PubMed

Chen, Fengli; Jia, Jia; Zhang, Qiang; Gu, Huiyan; Yang, Lei

2017-11-17

In this work, a modified technique was developed to separate essential oil from the fruit of Amorpha fruticosa using microwave-assisted hydrodistillation concatenated liquid-liquid extraction (MHD-LLE). The new apparatus consists of two series-wound separation columns for separating essential oil, one is the conventional oil-water separation column, and the other is the extraction column of components from hydrosol using an organic solvent. Therefore, the apparatus can simultaneously collect the essential oil separated on the top of hydrosol and the components extracted from hydrosol using an organic solvent. Based on the yield of essential oil in the first and second separation columns, the effects of parameters were investigated by single factor experiments and Box-Behnken design. Under the optimum conditions (2mL ethyl ether as the extraction solvent in the second separation column, 12mL/g liquid-solid ratio, 4.0min homogenate time, 35min microwave irradiation time and 540W microwave irradiation power), satisfactory yields for the essential oil in the first separation column (10.31±0.33g/kg) and second separation column (0.82±0.03g/kg) were obtained. Compared with traditional methods, the developed method gave a higher yield of essential oil in a shorter time. In addition, GC-MS analysis of the essential oil indicated significant differences of the relative contents of individual volatile components in the essential oils obtained in the two separation columns. Therefore, the MHD-LLE technique developed here is a good alternative for the isolation of essential oil from A. fruticosa fruit as well as other herbs. Copyright © 2017 Elsevier B.V. All rights reserved.

Chiral separation of the β2-sympathomimetic fenoterol by HPLC and capillary zone electrophoresis for pharmacokinetic studies.

PubMed

Ullrich, Thomas; Wesenberg, Dirk; Bleuel, Corinna; Krauss, Gerd-Joachim; Schmid, Martin G; Weiss, Michael; Gübitz, Gerald

2010-10-01

The development of methods for the separation of the enantiomers of fenoterol by chiral HPLC and capillary zone electrophoresis (CZE) is described. For the HPLC separation precolumn fluorescence derivatization with naphthyl isocyanate was applied. The resulting urea derivatives were resolved on a cellulose tris(3,5-dimethylphenylcarbamate)-coated silica gel column employing a column switching procedure. Detection was carried out fluorimetrically with a detection limit in the low ng/mL range. The method was adapted to the determination of fenoterol enantiomers in rat heart perfusates using liquid-liquid extraction. As an alternative a CE method was used for the direct separation of fenoterol enantiomers comparing different cyclodextrin derivatives as chiral selectors. Copyright © 2010 John Wiley & Sons, Ltd.

Characterization of cellulose acetates according to DS and molar mass using two-dimensional chromatography.

PubMed

Ghareeb, Hewa Othman; Radke, Wolfgang

2013-11-06

A two-dimensional liquid chromatographic method (2D LC) was developed to analyze the heterogeneities of cellulose acetates (CA) in the DS-range DS=1.5-2.9 with respect to both, molar mass and degree of substitution (DS). The method uses gradient liquid chromatography (HPLC) as the first dimension in order to separate by DS followed by separation of the different fractions by size (SEC) in the second dimension. The 2D experiments revealed different correlations between gradient and SEC elution volume. These correlations might arise from differences in the synthetic conditions. The newly developed 2D LC separation therefore provides new insights into the heterogeneity of CAs. Copyright © 2013 Elsevier Ltd. All rights reserved.

Investigation of Super*Zip separation joint

NASA Technical Reports Server (NTRS)

Bement, Laurence J.; Schimmel, Morry L.

1988-01-01

An investigation to determine the most likely cause of two failures of five tests on 79 inch diameter Lockheed Super*Zip spacecraft separation joints being used for the development of a Shuttle/Centaur propulsion system. This joint utilizes an explosively expanded tube to fracture surrounding prenotched aluminum plates to achieve planar separation. A test method was developed and more than 300 tests firings were made to provide an understanding of severance mechanisms and the functional performance effects of system variables. An approach for defining functional margin was developed, and specific recommendations were made for improving existing and future systems.

Use of information entropy measures of sitting postural sway to quantify developmental delay in infants

PubMed Central

Deffeyes, Joan E; Harbourne, Regina T; DeJong, Stacey L; Kyvelidou, Anastasia; Stuberg, Wayne A; Stergiou, Nicholas

2009-01-01

Background By quantifying the information entropy of postural sway data, the complexity of the postural movement of different populations can be assessed, giving insight into pathologic motor control functioning. Methods In this study, developmental delay of motor control function in infants was assessed by analysis of sitting postural sway data acquired from force plate center of pressure measurements. Two types of entropy measures were used: symbolic entropy, including a new asymmetric symbolic entropy measure, and approximate entropy, a more widely used entropy measure. For each method of analysis, parameters were adjusted to optimize the separation of the results from the infants with delayed development from infants with typical development. Results The method that gave the widest separation between the populations was the asymmetric symbolic entropy method, which we developed by modification of the symbolic entropy algorithm. The approximate entropy algorithm also performed well, using parameters optimized for the infant sitting data. The infants with delayed development were found to have less complex patterns of postural sway in the medial-lateral direction, and were found to have different left-right symmetry in their postural sway, as compared to typically developing infants. Conclusion The results of this study indicate that optimization of the entropy algorithm for infant sitting postural sway data can greatly improve the ability to separate the infants with developmental delay from typically developing infants. PMID:19671183

Separation of Zirconium and Hafnium: A Review

NASA Astrophysics Data System (ADS)

Xu, L.; Xiao, Y.; van Sandwijk, A.; Xu, Q.; Yang, Y.

Zirconium is an ideal material for nuclear reactors due to its low absorption cross-section for thermal neutrons, whereas the typically contained hafnium with strong neutron-absorption is very harmful for zirconium. This paper provides an overview of the processes for separating hafnium from zirconium. The separation processes are roughly classified into hydro- and pyrometallurgical routes. The current dominant zirconium production route involves pyrometallurgical ore cracking, multi-step hydrometallurgical liquid-liquid extraction for hafnium removal and the reduction of zirconium tetrachloride to the pure metal by the Kroll process. The lengthy hydrometallurgical Zr-Hf separation operations leads to high production cost, intensive labour and heavy environmental burden. Using a compact pyrometallurgical separation method can simplify the whole production flowsheet with a higher process efficiency. The known separation methods are discussed based on the following reaction features: redox characteristics, volatility, electrochemical properties and molten salt extraction. The commercially operating extractive distillation process is a significant advance in Zr-Hf separation technology but it suffers from high process maintenance cost. The recently developed new process based on molten salt-metal equilibrium for Zr-Hf separation shows a great potential for industrial application, which is compact for nuclear grade zirconium production starting from crude ore. In the present paper, the available separation technologies are compared. The advantages and disadvantages as well as future directions of research and development for nuclear grade zirconium production are discussed.

Separation and reconstruction of BCG and EEG signals during continuous EEG and fMRI recordings

PubMed Central

Xia, Hongjing; Ruan, Dan; Cohen, Mark S.

2014-01-01

Despite considerable effort to remove it, the ballistocardiogram (BCG) remains a major artifact in electroencephalographic data (EEG) acquired inside magnetic resonance imaging (MRI) scanners, particularly in continuous (as opposed to event-related) recordings. In this study, we have developed a new Direct Recording Prior Encoding (DRPE) method to extract and separate the BCG and EEG components from contaminated signals, and have demonstrated its performance by comparing it quantitatively to the popular Optimal Basis Set (OBS) method. Our modified recording configuration allows us to obtain representative bases of the BCG- and EEG-only signals. Further, we have developed an optimization-based reconstruction approach to maximally incorporate prior knowledge of the BCG/EEG subspaces, and of the signal characteristics within them. Both OBS and DRPE methods were tested with experimental data, and compared quantitatively using cross-validation. In the challenging continuous EEG studies, DRPE outperforms the OBS method by nearly sevenfold in separating the continuous BCG and EEG signals. PMID:25002836

Validated Chromatographic Methods for the Analysis of Two Binary Mixtures Containing Pyridoxine Hydrochloride.

PubMed

Habib, Neven M; Abdelrahman, Maha M; Abdelwhab, Nada S; Ali, Nourudin W

2017-03-01

Accurate and precise TLC-densitometric and HPLC-diode-array detector (DAD) methods have been developed and validated to resolve two binary mixtures containing pyridoxine hydrochloride (PYH) with either cyclizine hydrochloride (CYH) or meclizine hydrochloride (MEH). In the developed TLC-densitometric method, chromatographic separation of the three studied drugs was carried out on silica gel 60 F254 plates using a developing system containing methylene chloride + acetone + methanol (7 + 1 + 0.5, v/v/v) scanning separated bands at 220 nm. Beer-Lambert law was obeyed in the ranges of 0.2-5, 0.2-4, and 0.2-4 µg/band for PYH, CYH, and MEH, respectively. On the other hand, the developed HPLC-DAD method depended on chromatographic separation on a Zorbax Eclipse C18 column using methanol-KH2PO4 (0.05 M; 90 + 10, v/v; pH 5, with H3PO4 and KOH) as the mobile phase, a flow rate of 1 mL/min, and UV scanning at 220 nm. A linear relationship was obtained between the integrated peak area and the concentration in the ranges of 10-50, 10-50, and 7-50 µg/mL for PYH, CYH, and MEH, respectively. The proposed methods were successfully applied for the determination of the cited drugs in their pharmaceutical formulations. Statistical comparison with the reported methods using Student's t- and F-tests found there were no significant differences between the proposed and reported methods for accuracy and precision.

DEVELOPMENT OF LOW-DIFFUSION FLUX-SPLITTING METHODS FOR DENSE GAS-SOLID FLOWS

EPA Science Inventory

The development of a class of low-diffusion upwinding methods for computing dense gas-solid flows is presented in this work. An artificial compressibility/low-Mach preconditioning strategy is developed for a hyperbolic two-phase flow equation system consisting of separate solids ...

Wet separation processes as method to separate limestone and oil shale

NASA Astrophysics Data System (ADS)

Nurme, Martin; Karu, Veiko

2015-04-01

Biggest oil shale industry is located in Estonia. Oil shale usage is mainly for electricity generation, shale oil generation and cement production. All these processes need certain quality oil shale. Oil shale seam have interlayer limestone layers. To use oil shale in production, it is needed to separate oil shale and limestone. A key challenge is find separation process when we can get the best quality for all product types. In oil shale separation typically has been used heavy media separation process. There are tested also different types of separation processes before: wet separation, pneumatic separation. Now oil shale industry moves more to oil production and this needs innovation methods for separation to ensure fuel quality and the changes in quality. The pilot unit test with Allmineral ALLJIG have pointed out that the suitable new innovation way for oil shale separation can be wet separation with gravity, where material by pulsating water forming layers of grains according to their density and subsequently separates the heavy material (limestone) from the stratified material (oil shale)bed. Main aim of this research is to find the suitable separation process for oil shale, that the products have highest quality. The expected results can be used also for developing separation processes for phosphorite rock or all others, where traditional separation processes doesn't work property. This research is part of the study Sustainable and environmentally acceptable Oil shale mining No. 3.2.0501.11-0025 http://mi.ttu.ee/etp and the project B36 Extraction and processing of rock with selective methods - http://mi.ttu.ee/separation; http://mi.ttu.ee/miningwaste/

Characterization of free thiol variants of an IgG1 by reversed phase ultra high pressure liquid chromatography coupled with mass spectrometry.

PubMed

Liu, Hongbin; Jeong, Justin; Kao, Yung-Hsiang; Zhang, Yonghua Taylor

2015-05-10

RP-HPLC has been demonstrated as a powerful tool to study antibody free thiol and disulfide variants. Recently, the introduction of UHPLC columns with wide pore size (300Å) and small particle size (1.7μm) offered the opportunity to further improve the separation of such variants. This paper describes a systematic evaluation of stationary phases, operating parameters, and mobile phases for a UHPLC based method to separate free thiol variants of a recombinant monoclonal antibody (referred as mAb A), targeting high resolution, high throughput and improved recovery. Among the four different stationary phases evaluated, UHPLC diphenyl columns were found to provide the best separation. Using an optimized UHPLC method, free thiol variants of mAb A were separated in 5min. Importantly, the UHPLC method revealed minor variants that had coeluted in an HPLC based method, and the UHPLC method is also applicable as a platform method for characterization of other mAbs as well. Furthermore, an on-line UHPLC-MS method was developed to characterize the separated variants, and this method can streamline the characterization of fully assembled monoclonal and bispecific therapeutic antibodies. Copyright © 2015 Elsevier B.V. All rights reserved.

Thin-layer chromatography with stationary phase gradient as a method for separation of water-soluble vitamins.

PubMed

Cimpoiu, Claudia; Hosu, Anamaria; Puscas, Anitta

2012-02-03

The group of hydrophilic vitamins play an important role in human health, and their lack or excess produces specific diseases. Therefore, the analysis of these compounds is indispensable for monitoring their content in pharmaceuticals and food in order to prevent some human diseases. TLC was successfully applied in the analysis of hydrophilic vitamins, but the most difficult problem in the simultaneous analysis of all these compounds is to find an optimum stationary phase-mobile phase system due to different chemical characteristics of analytes. Unfortunately structural analogues are difficult to separate in one chromatographic run, and this is the case in hydrophilic vitamins investigations. TLC gives the possibility to perform two-dimensional separations by using stationary phase gradient achieving the highest resolution by combining two systems with different selectivity. The goal of this work was to develop a method of analysis enabling separation of hydrophilic vitamins using TLC with adsorbent gradient. The developed method was used for identifying the water-soluble vitamins in alcoholic extracts of Hippophae rhamnoides and of Ribes nigrum. Copyright © 2011 Elsevier B.V. All rights reserved.

Optimization and development of a SPE-HPLC-UV method to determine astaxanthin in Saccharina japonica.

PubMed

Zhou, Jun; Bi, Wentao; Row, Kyung Ho

2011-04-01

An effective and accurate method including extraction, saponification, and separation was developed to determine astaxanthin (AX) in Saccharina japonica. The optimal extraction conditions with different solvents were investigated. 29.30 μg/g of AX was extracted from dry Saccharina japonica powder by solvent. After subsequent saponification, the extracted amount of AX was increased to 37.26 μg/g. Furthermore, 3 different ionic liquid-based silicas were prepared as sorbents for the solid phase extraction of AX from the extract. By comparing the adsorption isotherms of AX on different ionic liquid-based silicas, suitable sorbent was successfully selected and applied for separation of AX from extract. Astaxanthin, in 3 main forms (free, monoesters, and diesters), can be obtained from marine plants and animals. By extraction with subsequent saponification, the astaxanthin was extracted from Saccharina japonica. And then, ionic liquid-based silicas were used to separate the astaxanthin from the extract solution. This method can be widely applied for determination, or even industrial separation and purification of astaxanthin from many other algae.

Comparison of sampling methods for radiocarbon dating of carbonyls in air samples via accelerator mass spectrometry

NASA Astrophysics Data System (ADS)

Schindler, Matthias; Kretschmer, Wolfgang; Scharf, Andreas; Tschekalinskij, Alexander

2016-05-01

Three new methods to sample and prepare various carbonyl compounds for radiocarbon measurements were developed and tested. Two of these procedures utilized the Strecker synthetic method to form amino acids from carbonyl compounds with either sodium cyanide or trimethylsilyl cyanide. The third procedure used semicarbazide to form crystalline carbazones with the carbonyl compounds. The resulting amino acids and semicarbazones were then separated and purified using thin layer chromatography. The separated compounds were then combusted to CO2 and reduced to graphite to determine 14C content by accelerator mass spectrometry (AMS). All of these methods were also compared with the standard carbonyl compound sampling method wherein a compound is derivatized with 2,4-dinitrophenylhydrazine and then separated by high-performance liquid chromatography (HPLC).

The laboratory technology of discrete molecular separation: the historical development of gel electrophoresis and the material epistemology of biomolecular science, 1945-1970.

PubMed

Chiang, Howard Hsueh-hao

2009-01-01

Preparative and analytical methods developed by separation scientists have played an important role in the history of molecular biology. One such early method is gel electrophoresis, a technique that uses various types of gel as its supporting medium to separate charged molecules based on size and other properties. Historians of science, however, have only recently begun to pay closer attention to this material epistemological dimension of biomolecular science. This paper substantiates the historiographical thread that explores the relationship between modern laboratory practice and the production of scientific knowledge. It traces the historical development of gel electrophoresis from the mid-1940s to the mid-1960s, with careful attention to the interplay between technical developments and disciplinary shifts, especially the rise of molecular biology in this time-frame. Claiming that the early 1950s marked a decisive shift in the evolution of electrophoretic methods from moving boundary to zone electrophoresis, I reconstruct various trajectories in which scientists such as Oliver Smithies sought out the most desirable solid supporting medium for electrophoretic instrumentation. Biomolecular knowledge, I argue, emerged in part from this process of seeking the most appropriate supporting medium that allowed for discrete molecular separation and visualization. The early 1950s, therefore, marked not only an important turning point in the history of separation science, but also a transformative moment in the history of the life sciences as the growth of molecular biology depended in part on the epistemological access to the molecular realm available through these evolving technologies.

Comparison of originator and biosimilar therapeutic monoclonal antibodies using comprehensive two-dimensional liquid chromatography coupled with time-of-flight mass spectrometry.

PubMed

Sorensen, Matthew; Harmes, David C; Stoll, Dwight R; Staples, Gregory O; Fekete, Szabolcs; Guillarme, Davy; Beck, Alain

2016-10-01

As research, development, and manufacturing of biosimilar protein therapeutics proliferates, there is great interest in the continued development of a portfolio of complementary analytical methods that can be used to efficiently and effectively characterize biosimilar candidate materials relative to the respective reference (i.e., originator) molecule. Liquid phase separation techniques such as liquid chromatography and capillary electrophoresis are powerful tools that can provide both qualitative and quantitative information about similarities and differences between reference and biosimilar materials, especially when coupled with mass spectrometry. However, the inherent complexity of these protein materials challenges even the most modern one-dimensional (1D) separation methods. Two-dimensional (2D) separations present a number of potential advantages over 1D methods, including increased peak capacity, 2D peak patterns that can facilitate unknown identification, and improvement in the compatibility of some separation methods with mass spectrometry. In this study, we demonstrate the use of comprehensive 2D-LC separations involving cation-exchange (CEX) and reversed-phase (RP) separations in the first and second dimensions to compare 3 reference/biosimilar pairs of monoclonal antibodies (cetuximab, trastuzumab and infliximab) that cover a range of similarity/disimilarity in a middle-up approach. The second dimension RP separations are coupled to time-of-flight mass spectrometry, which enables direct identification of features in the chromatograms obtained from mAbs digested with the IdeS enzyme, or digestion with IdeS followed by reduction with dithiothreitol. As many as 23 chemically unique mAb fragments were detected in a single sample. Our results demonstrate that these rich datasets enable facile assesment of the degree of similarity between reference and biosimilar materials.

QRS classification and spatial combination for robust heart rate detection in low-quality fetal ECG recordings.

PubMed

Warmerdam, G; Vullings, R; Van Pul, C; Andriessen, P; Oei, S G; Wijn, P

2013-01-01

Non-invasive fetal electrocardiography (ECG) can be used for prolonged monitoring of the fetal heart rate (FHR). However, the signal-to-noise-ratio (SNR) of non-invasive ECG recordings is often insufficient for reliable detection of the FHR. To overcome this problem, source separation techniques can be used to enhance the fetal ECG. This study uses a physiology-based source separation (PBSS) technique that has already been demonstrated to outperform widely used blind source separation techniques. Despite the relatively good performance of PBSS in enhancing the fetal ECG, PBSS is still susceptible to artifacts. In this study an augmented PBSS technique is developed to reduce the influence of artifacts. The performance of the developed method is compared to PBSS on multi-channel non-invasive fetal ECG recordings. Based on this comparison, the developed method is shown to outperform PBSS for the enhancement of the fetal ECG.

Dynamic acoustic field activated cell separation (DAFACS).

PubMed

Skotis, G D; Cumming, D R S; Roberts, J N; Riehle, M O; Bernassau, A L

2015-02-07

Advances in diagnostics, cell and stem cell technologies drive the development of application-specific tools for cell and particle separation. Acoustic micro-particle separation offers a promising avenue for high-throughput, label-free, high recovery, cell and particle separation and isolation in regenerative medicine. Here, we demonstrate a novel approach utilizing a dynamic acoustic field that is capable of separating an arbitrary size range of cells. We first demonstrate the method for the separation of particles with different diameters between 6 and 45 μm and secondly particles of different densities in a heterogeneous medium. The dynamic acoustic field is then used to separate dorsal root ganglion cells. The shearless, label-free and low damage characteristics make this method of manipulation particularly suited for biological applications. Advantages of using a dynamic acoustic field for the separation of cells include its inherent safety and biocompatibility, the possibility to operate over large distances (centimetres), high purity (ratio of particle population, up to 100%), and high efficiency (ratio of separated particles over total number of particles to separate, up to 100%).

Development of a sensitive and rapid method for rifampicin impurity analysis using supercritical fluid chromatography.

PubMed

Li, Wei; Wang, Jun; Yan, Zheng-Yu

2015-10-10

A novel simple, fast and efficient supercritical fluid chromatography (SFC) method was developed and compared with RPLC method for the separation and determination of impurities in rifampicin. The separation was performed using a packed diol column and a mobile phase B (modifier) consisting of methanol with 0.1% ammonium formate (w/v) and 2% water (v/v). Overall satisfactory resolutions and peak shapes for rifampicin quinone (RQ), rifampicin (RF), rifamycin SV (RSV), rifampicin N-oxide (RNO) and 3-formylrifamycinSV (3-FR) were obtained by optimization of the chromatography system. With gradient elution of mobile phase, all of the impurities and the active were separated within 4 min. Taking full advantage of features of SFC (such as particular selectivity, non-sloping baseline in gradient elution, and without injection solvent effects), the method was successfully used for determination of impurities in rifampicin, with more impurity peaks detected, better resolution achieved and much less analysis time needed compared with conventional reversed-phase liquid chromatography (RPLC) methods. Copyright © 2015 Elsevier B.V. All rights reserved.

Environmental and human monitoring of Americium-241 utilizing extraction chromatography and {alpha}-Spectrometry

DOE Office of Scientific and Technical Information (OSTI.GOV)

Goldstein, S.J.; Hensley, C.A.; Armenta, C.E.

1997-03-01

Recent developments in extraction chromatography have simplified the separation of americium from complex matrices in preparation for {alpha}-spectroscopy relative to traditional methods. Here we present results of procedures developed/adapted for water, air, and bioassay samples with less than 1 g of inorganic residue. Prior analytical methods required the use of a complex, multistage procedure for separation of americium from these matrices. The newer, simplified procedure requires only a single 2 mL extraction chromatographic separation for isolation of Am and lanthanides from other components of the sample. This method has been implemented on an extensive variety of `real` environmental and bioassaymore » samples from the Los Alamos area, and consistently reliable and accurate results with appropriate detection limits have been obtained. The new method increases analytical throughput by a factor of {approx}2 and decreases environmental hazards from acid and mixed-waste generation relative to the prior technique. Analytical accuracy, reproducibility, and reliability are also significantly improved over the more complex and laborious method used previously. 24 refs., 2 figs., 2 tabs.« less

Stability of spanwise-modulated flows behind backward-facing steps

NASA Astrophysics Data System (ADS)

Boiko, A. V.; Dovgal, A. V.; Sorokin, A. M.

2017-10-01

An overview and synthesis of researches on development of local vortical disturbances in laminar separated flows downstream of backward-facing steps, in which the velocity field depends essentially on two variables are given. Peculiarities of transition to turbulence in such spatially inhomogeneous separated zones are discussed. The experimental data are supplemented by the linear stability characteristics of model velocity profiles of the separated flow computed using both the classical local formulation and the nonlocal approach based on the Floquet theory for partial differential equations with periodic coefficients. The results clarify the response of the local separated flows to their modulation with stationary geometrical and temperature inhomogeneities. The results can be useful for the development of new methods of laminar separation control.

Task 2 Report: Algorithm Development and Performance Analysis

DTIC Science & Technology

1993-07-01

separated peaks ............................................. 39 7-16 Example ILGC data for schedule 3 phosphites showing an analysis method which integrates...more closely follows the baseline ................. 40 7-18 Example R.GC data for schedule 3 phosphites showing an analysis method resulting in unwanted...much of the ambiguity that can arise in GC/MS with trace environmental samples, for example. Correlated chromatography, on the other hand, separates the

Development of a gas chromatography method for the determination of isotretinoin and its degradation products in pharmaceuticals.

PubMed

Lima, Eliana Martins; Diniz, Danielle G Almeida; Antoniosi-Filho, Nelson R

2005-07-15

This paper describes the development of a gas chromatography (GC) method used for the assay of isotretinoin in its isolated form and in pharmaceutical formulations. Isotretinoin soft and hard gelatin capsules were prepared with various excipients. The performance of the proposed gas chromatography method was compared to that of traditional high performance liquid chromatography (HPLC) systems for this substance, and the GC parameters were established based on several preliminary tests, including thermal analysis of isotretinoin. Results showed that gas chromatography-flame ionization detector (GC-FID) exhibited a separation efficiency superior to that of HPLC, particularly for separating isotretinoin degradation products. This method was proven to be effectively applicable to stability evaluation assays of isotretinoin and isotretinoin based pharmaceuticals.

De-pulping and Seed Separation from Tumba ( Citrullus colocynthis) Fruit

NASA Astrophysics Data System (ADS)

Mudgal, Vishvambhar Dayal

2017-09-01

Tumba ( Citrullus colocynthis) contains spongy pulp in which seeds are embedded unevenly. Seeds contain about 26% fats and 13% protein. The process of seed separation is highly time consuming and labour intensive. Two weeks are required to separate its seeds with traditional methods. The developed prototype, for separating tumba seeds, mainly consists of chopper, de-pulping screw, barrel assembly and seed separation unit. The de-pulping screw and barrel assembly was divided in two sections i.e. conveying (feeding zone) and compression sections (de-pulping zone). The performance of developed machine was evaluated at different screw speed in the range of 40-100 rpm. Maximum pulp removal efficiency of 78.1% was achieved with screw speed of 60 rpm. Seed separation from the pulp was carried out by adding different chemicals. Use of sodium hydroxide and potassium hydroxide produced seed separation up to 99%.

Electromigrative separation techniques in forensic science: combining selectivity, sensitivity, and robustness.

PubMed

Posch, Tjorben Nils; Pütz, Michael; Martin, Nathalie; Huhn, Carolin

2015-01-01

In this review we introduce the advantages and limitations of electromigrative separation techniques in forensic toxicology. We thus present a summary of illustrative studies and our own experience in the field together with established methods from the German Federal Criminal Police Office rather than a complete survey. We focus on the analytical aspects of analytes' physicochemical characteristics (e.g. polarity, stereoisomers) and analytical challenges including matrix tolerance, separation from compounds present in large excess, sample volumes, and orthogonality. For these aspects we want to reveal the specific advantages over more traditional methods. Both detailed studies and profiling and screening studies are taken into account. Care was taken to nearly exclusively document well-validated methods outstanding for the analytical challenge discussed. Special attention was paid to aspects exclusive to electromigrative separation techniques, including the use of the mobility axis, the potential for on-site instrumentation, and the capillary format for immunoassays. The review concludes with an introductory guide to method development for different separation modes, presenting typical buffer systems as starting points for different analyte classes. The objective of this review is to provide an orientation for users in separation science considering using capillary electrophoresis in their laboratory in the future.

From Addition to Multiplication ... and Back: The Development of Students' Additive and Multiplicative Reasoning Skills

ERIC Educational Resources Information Center

Van Dooren, Wim; De Bock, Dirk; Verschaffel, Lieven

2010-01-01

This study builds on two lines of research that have so far developed largely separately: the use of additive methods to solve proportional word problems and the use of proportional methods to solve additive word problems. We investigated the development with age of both kinds of erroneous solution methods. We gave a test containing missing-value…

Alternative polymer separation technology by centrifugal force in a melted state

DOE Office of Scientific and Technical Information (OSTI.GOV)

Dobrovszky, Károly; Ronkay, Ferenc, E-mail: ronkay@pt.bme.hu

2014-11-15

Highlights: • Waste separation should take place at high purity. • Developed a novel, alternative separation method, where the separation occurred in a melted state by centrifugal forces. • Possibility of separation two different plastics into neat fractions. • High purity fractions were established at granulates and also at prefabricated blend. • Results were verified by DSC, optical microscopy and Raman spectroscopy. - Abstract: In order to upgrade polymer waste during recycling, separation should take place at high purity. The present research was aimed to develop a novel, alternative separation opportunity, where the polymer fractions were separated by centrifugal forcemore » in melted state. The efficiency of the constructed separation equipment was verified by two immiscible plastics (polyethylene terephthalate, PET; low density polyethylene, LDPE), which have a high difference of density, and of which large quantities can also be found in the municipal solid waste. The results show that the developed equipment is suitable not only for separating dry blended mixtures of PET/LDPE into pure components again, but also for separating prefabricated polymer blends. By this process it becomes possible to recover pure polymer substances from multi-component products during the recycling process. The adequacy of results was verified by differential scanning calorimetry (DSC) measurement as well as optical microscopy and Raman spectroscopy.« less

Separation of dietary omega-3 and omega-6 fatty acids in food by capillary electrophoresis.

PubMed

Soliman, Laiel C; Donkor, Kingsley K; Church, John S; Cinel, Bruno; Prema, Dipesh; Dugan, Michael E R

2013-10-01

A lower dietary omega-6/omega-3 (n-6/n-3) fatty acid ratio (<4) has been shown to be beneficial in preventing a number of chronic illnesses. Interest exists in developing more rapid and sensitive analytical methods for profiling fatty acid levels in foods. An aqueous CE method was developed for the simultaneous determination of 15 n-3 and n-6 relevant fatty acids. The effect of pH and concentration of buffer, type and concentration of organic modifier, and additive on the separation was investigated in order to determine the best conditions for the analysis. Baseline separations of the 15 fatty acids were achieved using 40 mM borate buffer at pH 9.50 containing 50 mM SDS, 10 mM β-cyclodextrin, and 10% acetonitrile. The developed CE method has LODs of <5 mg/L and good linearity (R(2) > 0.980) for all fatty acids studied. The proposed method was successfully applied to the determination of n-3 and n-6 fatty acids in flax seed, Udo® oils and a selection of grass-fed and grain-fed beef muscle samples. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Structure Optimization of a Grain Impact Piezoelectric Sensor and Its Application for Monitoring Separation Losses on Tangential-Axial Combine Harvesters

PubMed Central

Liang, Zhenwei; Li, Yaoming; Zhao, Zhan; Xu, Lizhang

2015-01-01

Grain separation losses is a key parameter to weigh the performance of combine harvesters, and also a dominant factor for automatically adjusting their major working parameters. The traditional separation losses monitoring method mainly rely on manual efforts, which require a high labor intensity. With recent advancements in sensor technology, electronics and computational processing power, this paper presents an indirect method for monitoring grain separation losses in tangential-axial combine harvesters in real-time. Firstly, we developed a mathematical monitoring model based on detailed comparative data analysis of different feeding quantities. Then, we developed a grain impact piezoelectric sensor utilizing a YT-5 piezoelectric ceramic as the sensing element, and a signal process circuit designed according to differences in voltage amplitude and rise time of collision signals. To improve the sensor performance, theoretical analysis was performed from a structural vibration point of view, and the optimal sensor structural has been selected. Grain collide experiments have shown that the sensor performance was greatly improved. Finally, we installed the sensor on a tangential-longitudinal axial combine harvester, and grain separation losses monitoring experiments were carried out in North China, which results have shown that the monitoring method was feasible, and the biggest measurement relative error was 4.63% when harvesting rice. PMID:25594592

Development of an analytical method for separation of phenolic acids by ultra-performance convergence chromatography (UPC2) using a column packed with a sub-2-μm particle.

PubMed

Jiang, Hai; Yang, Liu; Xing, Xudong; Yan, Meiling; Guo, Xinyue; Yang, Bingyou; Wang, Qiu-Hong; Kuang, Hai-Xue

2018-05-10

Phenolic acids are important active components of certain Traditional Chinese Medicines (TCM) and have a wide range of biological effects. Separation and purification of phenolic acids remains challenging due to difficulties with quality control using existing chromatographic methods The purpose of this study was to compare the effects of different chromatographic columns and conditions for the separation of phenolic acids. The BEH column was determined to be optimal, providing efficient separation in the shortest time (17.00 min) using gradient elution with carbon dioxide as the mobile phase, methanol/acetonitrile (70:30, v/v) with 1% TFA as the modifier, and a flow rate of 0.8 mL/min. Good peak shapes were obtained, and the peak asymmetry values were close to 1.00 for all phenolic acids. The resolution was more than 2.83 for all separated peaks. The developed method was subsequently applied to the determination of phenolic acids in Xanthii Fructus. These results are beneficial for quality control and standardization of herbal drugs using UPC 2 , providing an efficient, rapid and environmentally friendly scientific basis for future analysis of phenolic acids. Copyright © 2018. Published by Elsevier B.V.

Structure optimization of a grain impact piezoelectric sensor and its application for monitoring separation losses on tangential-axial combine harvesters.

PubMed

Liang, Zhenwei; Li, Yaoming; Zhao, Zhan; Xu, Lizhang

2015-01-14

Grain separation losses is a key parameter to weigh the performance of combine harvesters, and also a dominant factor for automatically adjusting their major working parameters. The traditional separation losses monitoring method mainly rely on manual efforts, which require a high labor intensity. With recent advancements in sensor technology, electronics and computational processing power, this paper presents an indirect method for monitoring grain separation losses in tangential-axial combine harvesters in real-time. Firstly, we developed a mathematical monitoring model based on detailed comparative data analysis of different feeding quantities. Then, we developed a grain impact piezoelectric sensor utilizing a YT-5 piezoelectric ceramic as the sensing element, and a signal process circuit designed according to differences in voltage amplitude and rise time of collision signals. To improve the sensor performance, theoretical analysis was performed from a structural vibration point of view, and the optimal sensor structural has been selected. Grain collide experiments have shown that the sensor performance was greatly improved. Finally, we installed the sensor on a tangential-longitudinal axial combine harvester, and grain separation losses monitoring experiments were carried out in North China, which results have shown that the monitoring method was feasible, and the biggest measurement relative error was 4.63% when harvesting rice.

Liquid chromatographic separation and thermodynamic investigation of lorcaserin hydrochloride enantiomers on immobilized amylose-based chiral stationary phase.

PubMed

Wani, Dattatraya V; Rane, Vipul P; Mokale, Santosh N

2018-03-01

A novel liquid chromatographic method was developed for enantiomeric separation of lorcaserin hydrochloride on Chiralpak IA column containing chiral stationary phase immobilized with amylose tris (3.5-dimethylphenylcarbamate) as chiral selector. Baseline separation with resolution greater than 4 was achieved using mobile phase containing mixture of n-hexane/ethanol/methanol/diethylamine (95:2.5:2.5:0.1, v/v/v/v) at a flow rate of 1.2 mL/min. The limit of detection and limit of quantification of the S-enantiomer were found to be 0.45 and 1.5 μg/mL, respectively; the developed method was validated as per ICH guideline. The influence of column oven temperatures studied in the range of 20°C to 50°C on separation was studied; from this, retention, separation, and resolution were investigated. The thermodynamic parameters ΔH°, ΔS°, and ΔG° were evaluated from van't Hoff plots,(Ink' versus 1/T) and used to explain the strength of interaction between enantiomers and immobilized amylose-based chiral stationary phase. © 2017 Wiley Periodicals, Inc.

Quality by design approach for the separation of naproxcinod and its related substances by fused core particle technology column.

PubMed

Inugala, Ugandar Reddy; Pothuraju, Nageswara Rao; Vangala, Ranga Reddy

2013-01-01

This paper describes the development of a rapid, novel, stability-indicating gradient reversed-phase high-performance liquid chromatographic method and associated system suitability parameters for the analysis of naproxcinod in the presence of its related substances and degradents using a quality-by-design approach. All of the factors that affect the separation of naproxcinod and its impurities and their mutual interactions were investigated and robustness of the method was ensured. The method was developed using an Ascentis Express C8 150 × 4.6 mm, 2.7 µm column with a mobile phase containing a gradient mixture of two solvents. The eluted compounds were monitored at 230 nm, the run time was 20 min within which naproxcinod and its eight impurities were satisfactorily separated. Naproxcinod was subjected to the stress conditions of oxidative, acid, base, hydrolytic, thermal and photolytic degradation. Naproxcinod was found to degrade significantly in acidic and basic conditions and to be stable in thermal, photolytic, oxidative and aqueous degradation conditions. The degradation products were satisfactorily resolved from the primary peak and its impurities, proving the stability-indicating power of the method. The developed method was validated as per International Conference on Harmonization guidelines with respect to specificity, linearity, limit of detection, limit of quantification, accuracy, precision and robustness.

An incremental block-line-Gauss-Seidel method for the Navier-Stokes equations

NASA Technical Reports Server (NTRS)

Napolitano, M.; Walters, R. W.

1985-01-01

A block-line-Gauss-Seidel (LGS) method is developed for solving the incompressible and compressible Navier-Stokes equations in two dimensions. The method requires only one block-tridiagonal solution process per iteration and is consequently faster per step than the linearized block-ADI methods. Results are presented for both incompressible and compressible separated flows: in all cases the proposed block-LGS method is more efficient than the block-ADI methods. Furthermore, for high Reynolds number weakly separated incompressible flow in a channel, which proved to be an impossible task for a block-ADI method, solutions have been obtained very efficiently by the new scheme.

Simultaneous separation by reversed-phase high-performance liquid chromatography and mass spectral identification of anthocyanins and flavonols in Shiraz grape skin.

PubMed

Downey, Mark O; Rochfort, Simone

2008-08-01

A limitation of large-scale viticultural trials is the time and cost of comprehensive compositional analysis of the fruit by high-performance liquid chromatography (HPLC). In addition, separate methods have generally been required to identify and quantify different classes of metabolites. To address these shortcomings a reversed-phase HPLC method was developed to simultaneously separate the anthocyanins and flavonols present in grape skins. The method employs a methanol and water gradient acidified with 10% formic acid with a run-time of 48 min including re-equilibration. Identity of anthocyanins and flavonols in Shiraz (Vitis vinifera L.) skin was confirmed by mass spectral analysis.

Separation membrane development

DOE Office of Scientific and Technical Information (OSTI.GOV)

Lee, M.W.

1998-08-01

A ceramic membrane has been developed to separate hydrogen from other gases. The method used is a sol-gel process. A thin layer of dense ceramic material is coated on a coarse ceramic filter substrate. The pore size distribution in the thin layer is controlled by a densification of the coating materials by heat treatment. The membrane has been tested by permeation measurement of the hydrogen and other gases. Selectivity of the membrane has been achieved to separate hydrogen from carbon monoxide. The permeation rate of hydrogen through the ceramic membrane was about 20 times larger than Pd-Ag membrane.

Analysis and characterization of heparin impurities.

PubMed

Beni, Szabolcs; Limtiaco, John F K; Larive, Cynthia K

2011-01-01

This review discusses recent developments in analytical methods available for the sensitive separation, detection and structural characterization of heparin contaminants. The adulteration of raw heparin with oversulfated chondroitin sulfate (OSCS) in 2007-2008 spawned a global crisis resulting in extensive revisions to the pharmacopeia monographs on heparin and prompting the FDA to recommend the development of additional physicochemical methods for the analysis of heparin purity. The analytical chemistry community quickly responded to this challenge, developing a wide variety of innovative approaches, several of which are reported in this special issue. This review provides an overview of methods of heparin isolation and digestion, discusses known heparin contaminants, including OSCS, and summarizes recent publications on heparin impurity analysis using sensors, near-IR, Raman, and NMR spectroscopy, as well as electrophoretic and chromatographic separations.

Separation of biogenic materials by electrophoresis under zero gravity (L-3)

NASA Technical Reports Server (NTRS)

Kuroda, Masao

1993-01-01

Electrophoresis separates electrically charged materials by imposing a voltage between electrodes. Though free-flow electrophoresis is used without carriers such as colloids to separate and purify biogenic materials including biogenic cells and proteins in blood, its resolving power and separation efficiency is very low on Earth due to sedimentation, flotation, and thermal convection caused by the specific gravity differences between separated materials and buffer solutions. The objective of this experiment is to make a comparative study of various electrophoresis conditions on the ground and in zero-gravity in order to ultimately develop a method for separating various important 'vial' components which are difficult to separate on the ground.

Use of a polystyrene-divinylbenzene-based weakly acidic cation-exchange resin column and propionic acid as an eluent in ion-exclusion/adsorption chromatography of aliphatic carboxylic acids and ethanol in food samples.

PubMed

Mori, Masanobu; Hironaga, Takahiro; Kajiwara, Hiroe; Nakatani, Nobutake; Kozaki, Daisuke; Itabashi, Hideyuki; Tanaka, Kazuhiko

2011-01-01

We developed an ion-exclusion/adsorption chromatography (IEAC) method employing a polystyrene-divinylbenzene-based weakly acidic cation-exchange resin (PS-WCX) column with propionic acid as the eluent for the simultaneous determination of multivalent aliphatic carboxylic acids and ethanol in food samples. The PS-WCX column well resolved mono-, di-, and trivalent carboxylic acids in the acidic eluent. Propionic acid as the eluent gave a higher signal-to-noise ratio, and enabled sensitive conductimetric detection of analyte acids. We found the optimal separation condition to be the combination of a PS-WCX column and 20-mM propionic acid. Practical applicability of the developed method was confirmed by using a short precolumn with a strongly acidic cation-exchange resin in the H(+)-form connected before the separation column; this was to remove cations from food samples by converting them to hydrogen ions. Consequently, common carboxylic acids and ethanol in beer, wine, and soy sauce were successfully separated by the developed method.

DEVELOPMENT AND VALIDATION OF AN ION CHROMATOGRAPHIC METHOD FOR DETERMINING PERCHLORATE IN FERTILIZERS

EPA Science Inventory

A method has been developed for the determination of perchlorate in fertilizers. Materials are leached with deionized water to dissolve any soluble perchlorate compounds. Ion chromatographic separation is followed by suppressed conductivity for detection. Perchlorate is retained ...

Prediction of antisymmetric buffet loads on horizontal stabilizers in massively separated flows, phase II

DOT National Transportation Integrated Search

1999-05-01

The Federal Aviation Administration (FAA) has a continuing program to collect data and develop predictive methods for aircraft flight loads. Some of the most severe and potentially catastrophic flight loads are produced by separated flows. Structural...

Sea level side loads in high-area-ratio rocket engines

NASA Technical Reports Server (NTRS)

Nave, L. H.; Coffey, G. A.

1973-01-01

An empirical separation and side load model to obtain applied aerodynamic loads has been developed based on data obtained from full-scale J-2S (265K-pound-thrust engine with an area ratio of 40:1) engine and model testing. Experimental data include visual observations of the separation patterns that show the dynamic nature of the separation phenomenon. Comparisons between measured and applied side loads are made. Correlations relating the separation location to the applied side loads and the methods used to determine the separation location are given.

Effects of Microwave Radiation on Oil Recovery

NASA Astrophysics Data System (ADS)

Esmaeili, Abdollah

2011-12-01

A variety of oil recovery methods have been developed and applied to mature and depleted reservoirs in order to improve the efficiency. Microwave radiation oil recovery method is a relatively new method and has been of great interest in the recent years. Crude oil is typically co-mingled with suspended solids and water. To increase oil recovery, it is necessary to remove these components. The separation of oil from water and solids using gravitational settling methods is typically incomplete. Oil-in-water and oil-water-solid emulsions can be demulsified and separated into their individual layers by microwave radiation. The data also show that microwave separation is faster than gravity separation and can be faster than conventional heating at many conditions. After separation of emulsion into water and oil layers, water can be discharged and oil is collected. High-frequency microwave recycling process can recover oil and gases from oil shale, residual oil, drill cuttings, tar sands oil, contaminated dredge/sediments, tires and plastics with significantly greater yields and lower costs than are available utilizing existing known technologies. This process is environmentally friendly, fuel-generating recycler to reduce waste, cut emissions, and save energy. This paper presents a critical review of Microwave radiation method for oil recovery.

Precipitation phase separation schemes in the Naqu River basin, eastern Tibetan plateau

NASA Astrophysics Data System (ADS)

Liu, Shaohua; Yan, Denghua; Qin, Tianling; Weng, Baisha; Lu, Yajing; Dong, Guoqiang; Gong, Boya

2018-01-01

Precipitation phase has a profound influence on the hydrological processes in the Naqu River basin, eastern Tibetan plateau. However, there are only six meteorological stations with precipitation phase (rainfall/snowfall/sleet) before 1979 within and around the basin. In order to separate snowfall from precipitation, a new separation scheme with S-shaped curve of snowfall proportion as an exponential function of daily mean temperature was developed. The determinations of critical temperatures in the single/two temperature threshold (STT/TTT2) methods were explored accordingly, and the temperature corresponding to the 50 % snowfall proportion (SP50 temperature) is an efficiently critical temperature for the STT, and two critical temperatures in TTT2 can be determined based on the exponential function and SP50 temperature. Then, different separation schemes were evaluated in separating snowfall from precipitation in the Naqu River basin. The results show that the S-shaped curve methods outperform other separation schemes. Although the STT and TTT2 slightly underestimate and overestimate the snowfall when the temperature is higher and colder than SP50 temperature respectively, the monthly and annual separation snowfalls are generally consistent with the observed snowfalls. On the whole, S-shaped curve methods, STT, and TTT2 perform well in separating snowfall from precipitation with the Pearson correlation coefficient of annual separation snowfall above 0.8 and provide possible approaches to separate the snowfall from precipitation for hydrological modelling.

Geological Sequestration Training and Research Program in Capture and Transport: Development of the Most Economical Separation Method for CO2 Capture

DOE Office of Scientific and Technical Information (OSTI.GOV)

Vahdat, Nader

2013-09-30

The project provided hands-on training and networking opportunities to undergraduate students in the area of carbon dioxide (CO2) capture and transport, through fundamental research study focused on advanced separation methods that can be applied to the capture of CO2 resulting from the combustion of fossil-fuels for power generation . The project team’s approach to achieve its objectives was to leverage existing Carbon Capture and Storage (CCS) course materials and teaching methods to create and implement an annual CCS short course for the Tuskegee University community; conduct a survey of CO2 separation and capture methods; utilize data to verify and developmore » computer models for CO2 capture and build CCS networks and hands-on training experiences. The objectives accomplished as a result of this project were: (1) A comprehensive survey of CO2 capture methods was conducted and mathematical models were developed to compare the potential economics of the different methods based on the total cost per year per unit of CO2 avoidance; and (2) Training was provided to introduce the latest CO2 capture technologies and deployment issues to the university community.« less

RAPID DETERMINATION OF ACTINIDES IN URINE BY INDUCTIVELY-COUPLED PLASMA MASS SPECTROMETRY AND ALPHA SPECTROMETRY: A HYBRID APPROACH

DOE Office of Scientific and Technical Information (OSTI.GOV)

Maxwell, S.; Jones, V.

2009-05-27

A new rapid separation method that allows separation and preconcentration of actinides in urine samples was developed for the measurement of longer lived actinides by inductively coupled plasma mass spectrometry (ICP-MS) and short-lived actinides by alpha spectrometry; a hybrid approach. This method uses stacked extraction chromatography cartridges and vacuum box technology to facilitate rapid separations. Preconcentration, if required, is performed using a streamlined calcium phosphate precipitation. Similar technology has been applied to separate actinides prior to measurement by alpha spectrometry, but this new method has been developed with elution reagents now compatible with ICP-MS as well. Purified solutions are splitmore » between ICP-MS and alpha spectrometry so that long- and short-lived actinide isotopes can be measured successfully. The method allows for simultaneous extraction of 24 samples (including QC samples) in less than 3 h. Simultaneous sample preparation can offer significant time savings over sequential sample preparation. For example, sequential sample preparation of 24 samples taking just 15 min each requires 6 h to complete. The simplicity and speed of this new method makes it attractive for radiological emergency response. If preconcentration is applied, the method is applicable to larger sample aliquots for occupational exposures as well. The chemical recoveries are typically greater than 90%, in contrast to other reported methods using flow injection separation techniques for urine samples where plutonium yields were 70-80%. This method allows measurement of both long-lived and short-lived actinide isotopes. 239Pu, 242Pu, 237Np, 243Am, 234U, 235U and 238U were measured by ICP-MS, while 236Pu, 238Pu, 239Pu, 241Am, 243Am and 244Cm were measured by alpha spectrometry. The method can also be adapted so that the separation of uranium isotopes for assay is not required, if uranium assay by direct dilution of the urine sample is preferred instead. Multiple vacuum box locations may be set-up to supply several ICP-MS units with purified sample fractions such that a high sample throughput may be achieved, while still allowing for rapid measurement of short-lived actinides by alpha spectrometry.« less

Enantioselective separation of all-E-astaxanthin and its determination in microbial sources.

PubMed

Grewe, Claudia; Menge, Sieglinde; Griehl, Carola

2007-09-28

A method for the enantioselective separation of all-E-astaxanthin (3,3'-dihydroxy-beta,beta-carotene-4,4'-dione), an important colorant in the feed industry, was developed. Different chiral stationary phases (CSPs) such as Pirkle phases (R,R Ulmo and l-leucine), modified polysaccharides and a beta-cyclodextrin have been investigated on their separation performance of astaxanthin enantiomers. Direct resolution was only achieved employing the Chiralcel OD-RH (cellulose-tris-3,5-dimethylphenyl-carbamate) under reversed phase conditions. The chiral separation of the enantiomeric forms of astaxanthin produced in microalgae and yeasts was reported. The yeast Xanthophyllomyces sp. produces astaxanthin predominantly in the R,R configuration, whereas in the green microalgae Scenedesmus sp. astaxanthin is built primarily in the S,S form. The separation method for the identification of astaxanthin enantiomers is of great interest since astaxanthin is used as functional food additive in human nutrition. Moreover the method may be used as a food chain indicator in farmed salmon.

Conjugates of magnetic nanoparticle-actinide specific chelator for radioactive waste separation.

PubMed

Kaur, Maninder; Zhang, Huijin; Martin, Leigh; Todd, Terry; Qiang, You

2013-01-01

A novel nanotechnology for the separation of radioactive waste that uses magnetic nanoparticles (MNPs) conjugated with actinide specific chelators (MNP-Che) is reviewed with a focus on design and process development. The MNP-Che separation process is an effective way of separating heat generating minor actinides (Np, Am, Cm) from spent nuclear fuel solution to reduce the radiological hazard. It utilizes coated MNPs to selectively adsorb the contaminants onto their surfaces, after which the loaded particles are collected using a magnetic field. The MNP-Che conjugates can be recycled by stripping contaminates into a separate, smaller volume of solution, and then become the final waste form for disposal after reusing number of times. Due to the highly selective chelators, this remediation method could be both simple and versatile while allowing the valuable actinides to be recovered and recycled. Key issues standing in the way of large-scale application are stability of the conjugates and their dispersion in solution to maintain their unique properties, especially large surface area, of MNPs. With substantial research progress made on MNPs and their surface functionalization, as well as development of environmentally benign chelators, this method could become very flexible and cost-effective for recycling used fuel. Finally, the development of this nanotechnology is summarized and its future direction is discussed.

Synthesis of amino-rich silica-coated magnetic nanoparticles for the efficient capture of DNA for PCR.

PubMed

Bai, Yalong; Cui, Yan; Paoli, George C; Shi, Chunlei; Wang, Dapeng; Zhou, Min; Zhang, Lida; Shi, Xianming

2016-09-01

Magnetic separation has great advantages over traditional bio-separation methods and has become popular in the development of methods for the detection of bacterial pathogens, viruses, and transgenic crops. Functionalization of magnetic nanoparticles is a key factor for efficient capture of the target analytes. In this paper, we report the synthesis of amino-rich silica-coated magnetic nanoparticles using a one-pot method. This type of magnetic nanoparticle has a rough surface and a higher density of amino groups than the nanoparticles prepared by a post-modification method. Furthermore, the results of hydrochloric acid treatment indicated that the magnetic nanoparticles were stably coated. The developed amino-rich silica-coated magnetic nanoparticles were used to directly adsorb DNA. After magnetic separation and blocking, the magnetic nanoparticles and DNA complexes were used directly for the polymerase chain reaction (PCR), without onerous and time-consuming purification and elution steps. The results of real-time quantitative PCR showed that the nanoparticles with higher amino group density resulted in improved DNA capture efficiency. The results suggest that amino-rich silica-coated magnetic nanoparticles are of great potential for efficient bio-separation of DNA prior to detection by PCR. Copyright © 2016. Published by Elsevier B.V.

Development of an on-line mixed-mode gel liquid chromatography×reversed phase liquid chromatography method for separation of water extract from Flos Carthami.

PubMed

Wang, Yu-Qing; Tang, Xu; Li, Jia-Fu; Wu, Yun-Long; Sun, Yu-Ying; Fang, Mei-Juan; Wu, Zhen; Wang, Xiu-Min; Qiu, Ying-Kun

2017-10-13

A novel on-line comprehensive two-dimensional liquid chromatography (2D-LC) method by coupling mixed-mode gel liquid chromatography (MMG-LC) with reversed phase liquid chromatography (RPLC) was developed. A mixture of 17 reference compounds was used to study the separation mechanism. A crude water extract of Flos Carthami was applied to evaluate the performance of the novel 2D-LC system. In the first dimension, the extract was eluted with a gradient of water/methanol over a cross-linked dextran gel Sephadex LH-20 column. Meanwhile, the advantages of size exclusion, reversed phase partition and adsorption separation mechanism were exploited before further on-line reversed phase purification on the second dimension. This novel on-line mixed-mode Sephadex LH-20×RPLC method provided higher peak resolution, sample processing ability (2.5mg) and better orthogonality (72.9%) versus RPLC×RPLC and hydrophilic interaction liquid chromatography (HILIC)×RPLC. To the best of our knowledge, this is the first report of a mixed-mode Sephadex LH-20×RPLC separation method with successful applications in on-line mode, which might be beneficial for harvesting targets from complicated medicinal plants. Copyright © 2017 Elsevier B.V. All rights reserved.

A dispersion relationship governing incompressible wall turbulence

NASA Technical Reports Server (NTRS)

Tsuge, S.

1978-01-01

The method of separation of variables is shown to make turbulent correlation equations of Karman-Howarth type tractable for shear turbulence as well under the condition of neglected triple correlation. The separated dependent variable obeys an Orr-Sommerfeld equation. A new analytical method is developed using a scaling law different from the classical one due to Heisenberg and Lin and more appropriate for wall turbulent profiles. A dispersion relationship between the wave number and the separation constant which has the dimension of a frequency is derived in support of experimental observations of wave or coherent structure of wall turbulence.

Active Solvent Modulation: A Valve-Based Approach To Improve Separation Compatibility in Two-Dimensional Liquid Chromatography.

PubMed

Stoll, Dwight R; Shoykhet, Konstantin; Petersson, Patrik; Buckenmaier, Stephan

2017-09-05

Two-dimensional liquid chromatography (2D-LC) is increasingly being viewed as a viable tool for solving difficult separation problems, ranging from targeted separations of structurally similar molecules to untargeted separations of highly complex mixtures. In spite of this performance potential, though, many users find method development challenging and most frequently cite the "incompatibility" between the solvent systems used in the first and second dimensions as a major obstacle. This solvent strength related incompatibility can lead to severe peak distortion and loss of resolution and sensitivity in the second dimension. In this paper, we describe a novel approach to address the incompatibility problem, which we refer to as Active Solvent Modulation (ASM). This valve-based approach enables dilution of 1 D effluent with weak solvent prior to transfer to the 2 D column but without the need for additional instrument hardware. ASM is related to the concept we refer to as Fixed Solvent Modulation (FSM), with the important difference being that ASM allows toggling of the diluent stream during each 2 D separation cycle. In this work, we show that ASM eliminates the major drawbacks of FSM including complex elution solvent profiles, baseline disturbances, and slow 2 D re-equilibration and demonstrate improvements in 2 D separation quality using both simple small molecule probes and degradants of heat-treated bovine insulin as case studies. We believe that ASM will significantly ease method development for 2D-LC, providing a path to practical methods that involve both highly complementary 1 D and 2 D separations and sensitive detection.

Improvement of pre-treatment method for 36Cl/Cl measurement of Cl in natural groundwater by AMS

NASA Astrophysics Data System (ADS)

Nakata, Kotaro; Hasegawa, Takuma

2011-02-01

Estimation of 36Cl/Cl by accelerator mass spectrometry (AMS) is a useful method to trace hydrological processes in groundwater. For accurate estimation, separation of SO42- from Cl - in groundwater is required because 36S affects AMS measurement of 36Cl. Previous studies utilized the difference in solubility between BaSO 4 and BaCl 2 (BaSO 4 method) to chemically separate SO42- from Cl -. However, the accuracy of the BaSO 4 method largely depends on operator skill, and consequently Cl - recovery is typically incomplete (70-80%). In addition, the method is time consuming (>1 week), and cannot be applied directly to dilute solutions. In this study, a method based on ion-exchange column chromatography (column method) was developed for separation of Cl - and SO42-. Optimum conditions were determined for the diameter and height of column, type and amount of resin, type and concentration of eluent, and flow rate. The recovery of Cl - was almost 100%, which allowed complete separation from SO42-. The separation procedure was short (<6 h), and was successfully applied to dilute (1 mg/L Cl) solution. Extracted pore water and diluted seawater samples were processed by the column and BaSO 4 methods, and then analyzed by AMS to estimate 36S counts and 36Cl/Cl values. 36S counts in samples processed by the column method were stable and lower than those from the BaSO 4 method. The column method has the following advantages over the BaSO 4 method: (1) complete and stable separation of Cl - and SO42-, (2) less operator influence on results, (3) short processing time (<6 h), (4) high (almost 100%) recovery of Cl -, and (5) concentration of Cl - and separation from SO42- in the one system for dilute solutions.

A simple and rapid technique for radiochemical separation of iodine radionuclides from irradiated tellurium using an activated charcoal column.

PubMed

Chattopadhyay, Sankha; Saha Das, Sujata

2009-10-01

A simple and inexpensive method for the separation of medically useful no-carrier-added (nca) iodine radionuclides from bulk amounts of irradiated tellurium dioxide (TeO(2)) target was developed. The beta(-) emitting (131)I radionuclide, produced by the decay of (131)Te through the (nat)Te(n, gamma)(131)Te nuclear reaction, was used for standardization of the radiochemical separation procedure. The radiochemical separation was performed by precipitation followed by column (activated charcoal) chromatography. Quantitative post-irradiation recovery of the TeO(2) target material (98-99%), in a form suitable for reuse in future irradiations, was achieved. The overall radiochemical yield for the complete separation of (131)I was 75-85% (n=8). The separated nca (131)I was of high, approximately 99%, radionuclidic and radiochemical purities and did not contain detectable amounts of the target material. This method can be adopted for the radiochemical separation of other different iodine radionuclides produced from tellurium matrices through cyclotron as well as reactor irradiation.

Label-free cell separation and sorting in microfluidic systems

PubMed Central

Gossett, Daniel R.; Weaver, Westbrook M.; Mach, Albert J.; Hur, Soojung Claire; Tse, Henry Tat Kwong; Lee, Wonhee; Amini, Hamed

2010-01-01

Cell separation and sorting are essential steps in cell biology research and in many diagnostic and therapeutic methods. Recently, there has been interest in methods which avoid the use of biochemical labels; numerous intrinsic biomarkers have been explored to identify cells including size, electrical polarizability, and hydrodynamic properties. This review highlights microfluidic techniques used for label-free discrimination and fractionation of cell populations. Microfluidic systems have been adopted to precisely handle single cells and interface with other tools for biochemical analysis. We analyzed many of these techniques, detailing their mode of separation, while concentrating on recent developments and evaluating their prospects for application. Furthermore, this was done from a perspective where inertial effects are considered important and general performance metrics were proposed which would ease comparison of reported technologies. Lastly, we assess the current state of these technologies and suggest directions which may make them more accessible. Figure A wide range of microfluidic technologies have been developed to separate and sort cells by taking advantage of differences in their intrinsic biophysical properties PMID:20419490

Separation of sunscreens in skincare creams using greener high-temperature liquid chromatography and subcritical water chromatography.

PubMed

Kapalavavi, B; Marple, R; Gamsky, C; Yang, Y

2012-04-01

In this study, high-temperature liquid chromatographic (HTLC) and subcritical water chromatographic (SBWC) separations of sunscreens contained in skincare creams were achieved at temperatures ranging from 90 to 250°C. The columns employed in this work include a ZirChrom-DiamondBond-C18, a XTerra MS C18 and a XBridge C18 column. The quantity of methanol consumed by the greener HTLC sunscreen methods developed in this project is significantly reduced although the HTLC separation at this stage is not as efficient as that achieved by traditional HPLC. SBWC separation of sunscreens was also achieved on the XTerra MS C18 and the XBridge C18 columns using pure water at 230-250°C. Methanol was eliminated in the SBWC methods developed in this study. © 2011 The Authors. ICS © 2011 Society of Cosmetic Scientists and the Société Française de Cosmétologie.

A theoretical investigation of the aerodynamics of low-aspect-ratio wings with partial leading-edge separation

NASA Technical Reports Server (NTRS)

Mehrotra, S. C.; Lan, C. E.

1978-01-01

A numerical method is developed to predict distributed and total aerodynamic characteristics for low aspect-ratio wings with partial leading-edge separation. The flow is assumed to be steady and inviscid. The wing boundary condition is formulated by the quasi-vortex-lattice method. The leading-edge separated vortices are represented by discrete free vortex elements which are aligned with the local velocity vector at mid-points to satisfy the force free condition. The wake behind the trailing-edge is also force free. The flow tangency boundary condition is satisfied on the wing, including the leading- and trailing-edges. Comparison of the predicted results with complete leading-edge separation has shown reasonably good agreement. For cases with partial leading-edge separation, the lift is found to be highly nonlinear with angle of attack.

Recovery of 131I from alkaline solution of n-irradiated tellurium target using a tiny Dowex-1 column.

PubMed

Chattopadhyay, Sankha; Saha Das, Sujata

2010-10-01

A simple and inexpensive ion-exchange chromatography method for the separation of medically useful no-carrier-added (nca) iodine radionuclides from bulk amounts of irradiated tellurium dioxide (TeO(2)) target was developed and tested using (131)I. The radiochemical separation was performed using a very small Dowex-1x8 ion-exchange column. The overall radiochemical yield for the complete separation of (131)I was 92+/-1.8 (standard deviation) % (n=8). The separated nca (131)I was of high, approximately 99%, radionuclidic and radiochemical purity and did not contain detectable amounts of the target material. This method may be adopted for the radiochemical separation of other different iodine radionuclides produced from tellurium matrices through cyclotron as well as reactor irradiation. Copyright 2010 Elsevier Ltd. All rights reserved.

The difference between laboratory and in-situ pixel-averaged emissivity: The effects on temperature-emissivity separation

NASA Technical Reports Server (NTRS)

Matsunaga, Tsuneo

1993-01-01

Advanced Spaceborne Thermal Emission and Reflection Radiometer (ASTER) is a Japanese future imaging sensor which has five channels in thermal infrared (TIR) region. To extract spectral emissivity information from ASTER and/or TIMS data, various temperature-emissivity (T-E) separation methods have been developed to date. Most of them require assumptions on surface emissivity, in which emissivity measured in a laboratory is often used instead of in-situ pixel-averaged emissivity. But if these two emissivities are different, accuracies of separated emissivity and surface temperature are reduced. In this study, the difference between laboratory and in-situ pixel-averaged emissivity and its effect on T-E separation are discussed. TIMS data of an area containing both rocks and vegetation were also processed to retrieve emissivity spectra using two T-E separation methods.

Separation and identification of neutral cereal lipids by normal phase high-performance liquid chromatography, using evaporative light-scattering and electrospray mass spectrometry for detection.

PubMed

Rocha, João M; Kalo, Paavo J; Ollilainen, Velimatti; Malcata, F Xavier

2010-04-30

A novel method was developed for the analysis of molecular species in neutral lipid classes, using separation by normal phase high-performance liquid chromatography, followed by detection by evaporative light-scattering and electrospray ionization tandem mass spectrometry. Monoacid standards, i.e. sterol esters, triacylglycerols, fatty acids, diacylglycerols, free sterols and monoacylglycerols, were separated to baseline on microbore 3 microm-silica gel columns. Complete or partial separation of molecular species in each lipid class permitted identification by automatic tandem mass spectrometry of ammonium adducts, produced via positive electrospray ionization. After optimization of the method, separation and identification of molecular species of various lipid classes was comprehensively tested by analysis of neutral lipids from the free lipid extract of maize flour. 2010 Elsevier B.V. All rights reserved.

Protein Separation by Capillary Gel Electrophoresis: A Review

PubMed Central

Zhu, Zaifang; Lu, Joann J.; Liu, Shaorong

2011-01-01

Capillary gel electrophoresis (CGE) has been used for protein separation for more than two decades. Due to the technology advancement, current CGE methods are becoming more and more robust and reliable for protein analysis, and some of the methods have been routinely used for the analysis of protein-based pharmaceuticals and quality controls. In light of this progress, we survey 147 papers related to CGE separations of proteins and present an overview of this technology. We first introduce briefly the early development of CGE. We then review the methodology, in which we specifically describe the matrices, coatings, and detection strategies used in CGE. CGE using microfabricated channels and incorporation of CGE with two-dimensional protein separations are also discussed in this section. We finally present a few representative applications of CGE for separating proteins in real-world samples. PMID:22122927

Enhanced thermoelectric properties of phase-separating bismuth selenium telluride thin films via a two-step method

DOE Office of Scientific and Technical Information (OSTI.GOV)

Takashiri, Masayuki, E-mail: takashiri@tokai-u.jp; Kurita, Kensuke; Hagino, Harutoshi

2015-08-14

A two-step method that combines homogeneous electron beam (EB) irradiation and thermal annealing has been developed to enhance the thermoelectric properties of nanocrystalline bismuth selenium telluride thin films. The thin films, prepared using a flash evaporation method, were treated with EB irradiation in a N{sub 2} atmosphere at room temperature and an acceleration voltage of 0.17 MeV. Thermal annealing was performed under Ar/H{sub 2} (5%) at 300 °C for 60 min. X-ray diffraction was used to determine that compositional phase separation between bismuth telluride and bismuth selenium telluride developed in the thin films exposed to higher EB doses and thermal annealing. We proposemore » that the phase separation was induced by fluctuations in the distribution of selenium atoms after EB irradiation, followed by the migration of selenium atoms to more stable sites during thermal annealing. As a result, thin film crystallinity improved and mobility was significantly enhanced. This indicates that the phase separation resulting from the two-step method enhanced, rather than disturbed, the electron transport. Both the electrical conductivity and the Seebeck coefficient were improved following the two-step method. Consequently, the power factor of thin films that underwent the two-step method was enhanced to 20 times (from 0.96 to 21.0 μW/(cm K{sup 2}) that of the thin films treated with EB irradiation alone.« less

A new diagnostic method for separating airborne and structureborne noise radiated by plates with applications for propeller driven aircraft

NASA Technical Reports Server (NTRS)

Mcgary, Michael C.

1988-01-01

The anticipated application of advanced turboprop propulsion systems is expected to increase the interior noise of future aircraft to unacceptably high levels. The absence of technically and economically feasible noise source-path diagnostic tools has been a prime obstacle in the development of efficient noise control treatments for propeller-driven aircraft. A new diagnostic method that permits the separation and prediction of the fully coherent airborne and structureborne components of the sound radiated by plates or thin shells has been developed. Analytical and experimental studies of the proposed method were performed on an aluminum plate. The results of the study indicate that the proposed method could be used in flight, and has fewer encumbrances than the other diagnostic tools currently available.

Production of nuclear grade zirconium: A review

NASA Astrophysics Data System (ADS)

Xu, L.; Xiao, Y.; van Sandwijk, A.; Xu, Q.; Yang, Y.

2015-11-01

Zirconium is an ideal material for nuclear reactors due to its low absorption cross-section for thermal neutrons, whereas the typically contained hafnium with strong neutron-absorption is very harmful for zirconium as a fuel cladding material. This paper provides an overview of the processes for nuclear grade zirconium production with emphasis on the methods of Zr-Hf separation. The separation processes are roughly classified into hydro- and pyrometallurgical routes. The known pyrometallurgical Zr-Hf separation methods are discussed based on the following reaction features: redox characteristics, volatility, electrochemical properties and molten salt-metal equilibrium. In the present paper, the available Zr-Hf separation technologies are compared. The advantages and disadvantages as well as future directions of research and development for nuclear grade zirconium production are discussed.

Enhancing the Detection of Giardia duodenalis Cysts in Foods by Inertial Microfluidic Separation

PubMed Central

Ganz, Kyle R.; Clime, Liviu; Farber, Jeffrey M.; Corneau, Nathalie

2015-01-01

The sensitivity and specificity of current Giardia cyst detection methods for foods are largely determined by the effectiveness of the elution, separation, and concentration methods used. The aim of these methods is to produce a final suspension with an adequate concentration of Giardia cysts for detection and a low concentration of interfering food debris. In the present study, a microfluidic device, which makes use of inertial separation, was designed and fabricated for the separation of Giardia cysts. A cyclical pumping platform and protocol was developed to concentrate 10-ml suspensions down to less than 1 ml. Tests involving Giardia duodenalis cysts and 1.90-μm microbeads in pure suspensions demonstrated the specificity of the microfluidic chip for cysts over smaller nonspecific particles. As the suspension cycled through the chip, a large number of beads were removed (70%) and the majority of the cysts were concentrated (82%). Subsequently, the microfluidic inertial separation chip was integrated into a method for the detection of G. duodenalis cysts from lettuce samples. The method greatly reduced the concentration of background debris in the final suspensions (10-fold reduction) in comparison to that obtained by a conventional method. The method also recovered an average of 68.4% of cysts from 25-g lettuce samples and had a limit of detection (LOD) of 38 cysts. While the recovery of cysts by inertial separation was slightly lower, and the LOD slightly higher, than with the conventional method, the sample analysis time was greatly reduced, as there were far fewer background food particles interfering with the detection of cysts by immunofluorescence microscopy. PMID:25841016

Application of Silver Ion High-Performance Liquid Chromatography for Quantitative Analysis of Selected n-3 and n-6 PUFA in Oil Supplements.

PubMed

Czajkowska-Mysłek, Anna; Siekierko, Urszula; Gajewska, Magdalena

2016-04-01

The aim of this study was to develop a simple method for simultaneous determination of selected cis/cis PUFA-LNA (18:2), ALA (18:3), GLA (18:3), EPA (20:5), and DHA (22:6) by silver ion high-performance liquid chromatography coupled to a diode array detector (Ag-HPLC-DAD). The separation was performed on three Luna SCX Silver Loaded columns connected in series maintained at 10 °C with isocratic elution by 1% acetonitrile in n-hexane. The applied chromatographic system allowed a baseline separation of standard mixture of n-3 and n-6 fatty acid methyl esters containing LNA, DHA, and EPA and partial separation of ALA and GLA positional isomers. The method was validated by means of linearity, precision, stability, and recovery. Limits of detection (LOD) for considered PUFA standard solutions ranged from 0.27 to 0.43 mg L(-1). The developed method was used to evaluate of n-3 and n-6 fatty acids contents in plant and fish softgel oil capsules, results were compared with reference GC-FID based method.

Development and validation of a simple high-performance liquid chromatography analytical method for simultaneous determination of phytosterols, cholesterol and squalene in parenteral lipid emulsions.

PubMed

Novak, Ana; Gutiérrez-Zamora, Mercè; Domenech, Lluís; Suñé-Negre, Josep M; Miñarro, Montserrat; García-Montoya, Encarna; Llop, Josep M; Ticó, Josep R; Pérez-Lozano, Pilar

2018-02-01

A simple analytical method for simultaneous determination of phytosterols, cholesterol and squalene in lipid emulsions was developed owing to increased interest in their clinical effects. Method development was based on commonly used stationary (C 18 , C 8 and phenyl) and mobile phases (mixtures of acetonitrile, methanol and water) under isocratic conditions. Differences in stationary phases resulted in peak overlapping or coelution of different peaks. The best separation of all analyzed compounds was achieved on Zorbax Eclipse XDB C 8 (150 × 4.6 mm, 5 μm; Agilent) and ACN-H 2 O-MeOH, 80:19.5:0.5 (v/v/v). In order to achieve a shorter time of analysis, the method was further optimized and gradient separation was established. The optimized analytical method was validated and tested for routine use in lipid emulsion analyses. Copyright © 2017 John Wiley & Sons, Ltd.

SELECTIVE ENUMERATION OF AROMATIC AND ALIPHATIC HYDROCARBON DEGRADING BACTERIA BY A MOST-PROBABLE-NUMBER PROCEDURE

EPA Science Inventory

A most-portable-number (MPN) procedure was developed to separately enumerate aliphatic and aromatic hydrocarbon degrading bacteria, because most of the currently available methods are unable to distinguish between these two groups. Separate 96-well microtiter plates are used to ...

SEPARATION AND QUANTITATION OF NITROBENZENES AND THEIR REDUCTION PRODUCTS NITROANILINES AND PHENYLENEDIAMINES BY REVERSED=PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

EPA Science Inventory

A reversed-phase high-performance liquid chromatographic method for the separation and quantitation of a mixture consisting of nitrobenzene, dinitrobenzene isomers, 1,3,5-trinitrobenzene and their reduction products: aniline, nitroanilines and phenylenediamines has been developed...

Church-State Separation: Recent Trends and Developments.

ERIC Educational Resources Information Center

Sinensky, Jeffery P.; Kahn, Jill L.

1984-01-01

This report analyzes recent cases and legislation in the area of church-state separation. A brief introduction asserts that the Supreme Court's method of evaluating establishment clause controversies is undergoing pervasive changes that have permitted incursions on establishment principles. The rest of the paper, providing support for this…

Development of a Simple RP-HPLC-UV Method for Determination of Azithromycin in Bulk and Pharmaceutical Dosage forms as an Alternative to the USP Method

PubMed Central

Ghari, Tayebeh; Kobarfard, Farzad; Mortazavi, Seyed Alireza

2013-01-01

The present study was designed to develop a simple, validated liquid chromatographic method for the analysis of azithromycin in bulk and pharmaceutical dosage forms using ultraviolet detector. The best stationary phase was determined as C18 column, 5 μm, 250 mm × 4.6 mm. Mobile phase was optimized to obtain a fast and selective separation of the drug. Flow rate was 1.5 mL/min, Wavelength was set at 210 nm and the volume of each injection was 500 μL. An isocratic methanol/buffer mobile phase at the ratio of 90:10 v/v gave the best separation and resolution. The proposed method was accurate, precise, sensitive, and linear over a wide range of concentration of azithromycin. The developed method has the advantage of using UV detector compared to the USP method in which electrochemical detector has been used. The validated method was successfully applied to the determination of azithromycin in bulk and pharmaceutical dosage forms. PMID:24250672

Coulomb explosion: a novel approach to separate single-walled carbon nanotubes from their bundle.

PubMed

Liu, Guangtong; Zhao, Yuanchun; Zheng, Kaihong; Liu, Zheng; Ma, Wenjun; Ren, Yan; Xie, Sishen; Sun, Lianfeng

2009-01-01

A novel approach based on Coulomb explosion has been developed to separate single-walled carbon nanotubes (SWNTs) from their bundle. With this technique, we can readily separate a bundle of SWNTs into smaller bundles with uniform diameter as well as some individual SWNTs. The separated SWNTs have a typical length of several microns and form a nanotree at one end of the original bundle. More importantly, this separating procedure involves no surfactant and includes only one-step physical process. The separation method offers great conveniences for the subsequent individual SWNT or multiterminal SWNTs device fabrication and their physical properties studies.

Determination of free polysaccharide in Vi glycoconjugate vaccine against typhoid fever.

PubMed

Giannelli, C; Cappelletti, E; Di Benedetto, R; Pippi, F; Arcuri, M; Di Cioccio, V; Martin, L B; Saul, A; Micoli, F

2017-05-30

Glycoconjugate vaccines based on the Vi capsular polysaccharide directed against Salmonella enterica serovar Typhi are licensed or in development against typhoid fever, an important cause of morbidity and mortality in developing countries. Quantification of free polysaccharide in conjugate vaccines is an important quality control for release, to monitor vaccine stability and to ensure appropriate immune response. However, we found that existing separation methods based on size are not appropriate as free Vi non-specifically binds to unconjugated and conjugated protein. We developed a method based on free Vi separation by Capto Adhere resin and quantification by HPAEC-PAD. The method has been tested for conjugates of Vi derived from Citrobacter freundii with different carrier proteins such as CRM 197 , Tetanus Toxoid and Diphtheria Toxoid. Copyright © 2017 The Authors. Published by Elsevier B.V. All rights reserved.

A separable surface-enhanced Raman scattering substrate modified with MIL-101 for detection of overlapping and invisible compounds after thin-layer chromatography development.

PubMed

Zhang, Bin Bin; Shi, Yi; Chen, Hui; Zhu, Qing Xia; Lu, Feng; Li, Ying Wei

2018-01-02

By coupling surface-enhanced Raman spectroscopy (SERS) with thin-layer chromatography (TLC), a powerful method for detecting complex samples was successfully developed. However, in the TLC-SERS method, metal nanoparticles serving as the SERS-active substrate are likely to disturb the detection of target compounds, particularly in overlapping compounds after TLC development. In addition, the SERS detection of compounds that are invisible under both visible light and UV 254/365 after TLC development is still a significant challenge. In this study, we demonstrated a facile strategy to fabricate a TLC plate with metal-organic framework-modified gold nanoparticles as a separable SERS substrate, on which all separated components, including overlapping and invisible compounds, could be detected by a point-by-point SERS scan along the developing direction. Rhodamine 6G (R6G) was used as a probe to evaluate the performance of the substrate. The results indicated that the substrate provided good sensitivity and reproducibility, and optimal SERS signals could be collected in 5 s. Furthermore, this new substrate exhibited a long shelf life. Thus, our method has great potential for the sensitive and rapid detection of overlapping and invisible compounds in complex samples after TLC development. Copyright © 2017 The Author(s). Published by Elsevier B.V. All rights reserved.

Flow processes in overexpanded chemical rocket nozzles. Part 2: Side loads due to asymmetric separation

NASA Technical Reports Server (NTRS)

Schmucker, R. H.

1984-01-01

Methods for measuring the lateral forces, occurring as a result of asymmetric nozzle flow separation, are discussed. The effect of some parameters on the side load is explained. A new method was developed for calculation of the side load. The values calculated are compared with side load data of the J-2 engine. Results are used for predicting side loads of the space shuttle main engine.

Simultaneous separation and analysis of water- and fat-soluble vitamins on multi-modal reversed-phase weak anion exchange material by HPLC-UV.

PubMed

Dabre, Romain; Azad, Nazanin; Schwämmle, Achim; Lämmerhofer, Michael; Lindner, Wolfgang

2011-04-01

Several methods for the separation of vitamins on HPLC columns were already validated in the last 20 years. However, most of the techniques focus on separating either fat- or water-soluble vitamins and only few methods are intended to separate lipophilic and hydrophilic vitamins simultaneously. A mixed-mode reversed-phase weak anion exchange (RP-WAX) stationary phase was developed in our laboratory in order to address such mixture of analytes with different chemical characteristics, which are difficult to separate on standard columns. The high versatility in usage of the RP-WAX chromatographic material allowed a baseline separation of ten vitamins within a single run, seven water-soluble and three fat-soluble, using three different chromatographic modes: some positively charged vitamins are eluted in ion exclusion and ion repulsion modes whereas the negatively charged molecules are eluted in the ion exchange mechanism. The non-charged molecules are eluted in a classical reversed-phase mode, regarding their polarities. The method was validated for the vitamin analysis in tablets, evaluating selectivity, robustness, linearity, accuracy, and precision. The validated method was finally employed for the analysis of the vitamin content of some commercially available supplement tablets. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Novel methodology to isolate microplastics from vegetal-rich samples.

PubMed

Herrera, Alicia; Garrido-Amador, Paloma; Martínez, Ico; Samper, María Dolores; López-Martínez, Juan; Gómez, May; Packard, Theodore T

2018-04-01

Microplastics are small plastic particles, globally distributed throughout the oceans. To properly study them, all the methodologies for their sampling, extraction, and measurement should be standardized. For heterogeneous samples containing sediments, animal tissues and zooplankton, several procedures have been described. However, definitive methodologies for samples, rich in algae and plant material, have not yet been developed. The aim of this study was to find the best extraction protocol for vegetal-rich samples by comparing the efficacies of five previously described digestion methods, and a novel density separation method. A protocol using 96% ethanol for density separation was better than the five digestion methods tested, even better than using H 2 O 2 digestion. As it was the most efficient, simple, safe and inexpensive method for isolating microplastics from vegetal rich samples, we recommend it as a standard separation method. Copyright © 2018 Elsevier Ltd. All rights reserved.

Chiral separation of G-type chemical warfare nerve agents via analytical supercritical fluid chromatography.

PubMed

Kasten, Shane A; Zulli, Steven; Jones, Jonathan L; Dephillipo, Thomas; Cerasoli, Douglas M

2014-12-01

Chemical warfare nerve agents (CWNAs) are extremely toxic organophosphorus compounds that contain a chiral phosphorus center. Undirected synthesis of G-type CWNAs produces stereoisomers of tabun, sarin, soman, and cyclosarin (GA, GB, GD, and GF, respectively). Analytical-scale methods were developed using a supercritical fluid chromatography (SFC) system in tandem with a mass spectrometer for the separation, quantitation, and isolation of individual stereoisomers of GA, GB, GD, and GF. Screening various chiral stationary phases (CSPs) for the capacity to provide full baseline separation of the CWNAs revealed that a Regis WhelkO1 (SS) column was capable of separating the enantiomers of GA, GB, and GF, with elution of the P(+) enantiomer preceding elution of the corresponding P(-) enantiomer; two WhelkO1 (SS) columns had to be connected in series to achieve complete baseline resolution. The four diastereomers of GD were also resolved using two tandem WhelkO1 (SS) columns, with complete baseline separation of the two P(+) epimers. A single WhelkO1 (RR) column with inverse stereochemistry resulted in baseline separation of the GD P(-) epimers. The analytical methods described can be scaled to allow isolation of individual stereoisomers to assist in screening and development of countermeasures to organophosphorus nerve agents. © 2014 The Authors. Chirality published by John Wiley Periodicals, Inc.

Improved quality-by-design compliant methodology for method development in reversed-phase liquid chromatography.

PubMed

Debrus, Benjamin; Guillarme, Davy; Rudaz, Serge

2013-10-01

A complete strategy dedicated to quality-by-design (QbD) compliant method development using design of experiments (DOE), multiple linear regressions responses modelling and Monte Carlo simulations for error propagation was evaluated for liquid chromatography (LC). The proposed approach includes four main steps: (i) the initial screening of column chemistry, mobile phase pH and organic modifier, (ii) the selectivity optimization through changes in gradient time and mobile phase temperature, (iii) the adaptation of column geometry to reach sufficient resolution, and (iv) the robust resolution optimization and identification of the method design space. This procedure was employed to obtain a complex chromatographic separation of 15 antipsychotic basic drugs, widely prescribed. To fully automate and expedite the QbD method development procedure, short columns packed with sub-2 μm particles were employed, together with a UHPLC system possessing columns and solvents selection valves. Through this example, the possibilities of the proposed QbD method development workflow were exposed and the different steps of the automated strategy were critically discussed. A baseline separation of the mixture of antipsychotic drugs was achieved with an analysis time of less than 15 min and the robustness of the method was demonstrated simultaneously with the method development phase. Copyright © 2013 Elsevier B.V. All rights reserved.

Polymethacrylate-based monoliths as stationary phases for separation of biopolymers and immobilization of enzymes.

PubMed

Martinović, Tamara; Josić, Djuro

2017-11-01

The experiences in the production and application of polymethacrylate-based monolithic supports, since their development almost thirty years ago, are presented. The main driving force for the development of new chromatographic supports was the necessity for the isolation and separation of physiologically active biopolymers and their use for therapeutic purposes. For this sake, a development of a method for fast separation, preventing denaturation and preserving their biological activity was necessary. Development of polysaccharide-based supports, followed by the introduction of polymer-based chromatographic media, is shortly described. This development was followed by the advances in monolithic media that are now used for both large- and small-scale separation of biopolymers and nanoparticles. Finally, a short overview is given about the applications of monoliths for sample displacement chromatography, resulting in isolation of physiologically active biomolecules, such as proteins, protein complexes, and nucleic acid, as well as high-throughput sample preparation for proteomic investigations. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

High-performance liquid chromatography analysis methods developed for quantifying enzymatic esterification of flavonoids in ionic liquids.

PubMed

Lue, Bena-Marie; Guo, Zheng; Xu, Xuebing

2008-07-11

Methods using reversed-phase high-performance liquid chromatography (RP-HPLC) with ELSD were investigated to quantify enzymatic reactions of flavonoids with fatty acids in the presence of diverse room temperature ionic liquids (RTILs). A buffered salt (preferably triethylamine-acetate) was found essential for separation of flavonoids from strongly polar RTILs, whereby RTILs were generally visible as two major peaks identified based on an ion-pairing/exchanging hypothesis. C8 and C12 stationary phases were optimal while mobile phase pH (3-7) had only a minor influence on separation. The method developed was successfully applied for primary screening of RTILs (>20), with in depth evaluation of substrates in 10 RTILs, for their evaluation as reaction media.

Simultaneous determination of citrus limonoid aglycones and glucosides by high performance liquid chromatography.

PubMed

Vikram, Amit; Jayaprakasha, G K; Patil, Bhimanagouda S

2007-05-08

High performance liquid chromatography (HPLC) method has been developed for simultaneous quantification of limonoid aglycones and glucosides on a reversed phase C18 column using a binary solvent system, coupled with diode array detector. Seven limonoids such as limonin, nomilin, isolimonic acid, ichangin, isoobacunoic acid, limonin 17-beta-D glucopyranoside and deacetyl nomilinic acid 17-beta-D glucopyranoside were separated and detected at 210 nm. Furthermore, limonoids were separated, identified and quantified in four varieties of citrus fruits and seeds using developed method. Limonin and limonin glucoside were found to be the predominant limonoid aglycone and glucoside, respectively, in all tested samples. The sensitivity of the method was found to be 0.25-0.50 microg for tested limonoids.

Development of a High-Order Space-Time Matrix-Free Adjoint Solver

NASA Technical Reports Server (NTRS)

Ceze, Marco A.; Diosady, Laslo T.; Murman, Scott M.

2016-01-01

The growth in computational power and algorithm development in the past few decades has granted the science and engineering community the ability to simulate flows over complex geometries, thus making Computational Fluid Dynamics (CFD) tools indispensable in analysis and design. Currently, one of the pacing items limiting the utility of CFD for general problems is the prediction of unsteady turbulent ows.1{3 Reynolds-averaged Navier-Stokes (RANS) methods, which predict a time-invariant mean flowfield, struggle to provide consistent predictions when encountering even mild separation, such as the side-of-body separation at a wing-body junction. NASA's Transformative Tools and Technologies project is developing both numerical methods and physical modeling approaches to improve the prediction of separated flows. A major focus of this e ort is efficient methods for resolving the unsteady fluctuations occurring in these flows to provide valuable engineering data of the time-accurate flow field for buffet analysis, vortex shedding, etc. This approach encompasses unsteady RANS (URANS), large-eddy simulations (LES), and hybrid LES-RANS approaches such as Detached Eddy Simulations (DES). These unsteady approaches are inherently more expensive than traditional engineering RANS approaches, hence every e ort to mitigate this cost must be leveraged. Arguably, the most cost-effective approach to improve the efficiency of unsteady methods is the optimal placement of the spatial and temporal degrees of freedom (DOF) using solution-adaptive methods.

Interdisciplinary Methods in Water Resources

ERIC Educational Resources Information Center

Cosens, Barbara; Fiedler, Fritz; Boll, Jan; Higgins, Lorie; Johnson, Gary; Kennedy, Brian; Strand, Eva; Wilson, Patrick; Laflin, Maureen

2011-01-01

In the face of a myriad of complex water resource issues, traditional disciplinary separation is ineffective in developing approaches to promote a sustainable water future. As part of a new graduate program in water resources, faculty at the University of Idaho have developed a course on interdisciplinary methods designed to prepare students for…

Development of a temperature gradient focusing method for in situ extraterrestrial biomarker analysis.

PubMed

Danger, Grégoire; Ross, David

2008-08-01

Scanning temperature gradient focusing (TGF) is a recently described technique for the simultaneous concentration and separation of charged analytes. It allows for high analyte peak capacities and low LODs in microcolumn electrophoretic separations. In this paper, we present the application of scanning TGF for chiral separations of amino acids. Using a mixture of seven carboxyfluorescein succinimidyl ester-labeled amino acids (including five chiral amino acids) which constitute the Mars7 standard, we show that scanning TGF is a very simple and efficient method for chiral separations. The modulation of TGF separation parameters (temperature window, pressure scan rate, temperature range, and chiral selector concentration) allows optimization of peak efficiencies and analyte resolutions. The use of hydroxypropyl-beta-CD at low concentration (1-5 mmol/L) as a chiral selector, with an appropriate pressure scan rate ( -0.25 Pa/s) and with a low temperature range (3-25 degrees C over 1 cm) provided high resolution between enantiomers (Rs >1.5 for each pair of enantiomers) using a short, 4 cm long capillary. With these new results, the scanning TGF method appears to be a viable method for in situ trace biomarker analysis for future missions to Mars or other solar system bodies.

Enantiomeric separation and quantification of R/S-amphetamine in urine by ultra-high performance supercritical fluid chromatography tandem mass spectrometry.

PubMed

Hegstad, S; Havnen, H; Helland, A; Spigset, O; Frost, J

2018-03-01

To distinguish between legal and illegal consumption of amphetamine reliable analytical methods for chiral separation of the R- and S-enantiomers of amphetamine in biological specimens are required. In this regard, supercritical fluid chromatography (SFC) has several potential advantages over liquid chromatography, including rapid separation of enantiomers due to low viscosity and high diffusivity of supercritical carbon dioxide, the main component in the SFC mobile phase. A method for enantiomeric separation and quantification of R- and S-amphetamine in urine was developed and validated using ultra-high performance supercritical fluid chromatography-tandem mass spectrometry (UHPSFC-MS/MS). Sample preparation prior to UHPSFC-MS/MS analysis was a semi-automatic solid phase extraction method. The UHPSFC-MS/MS method used a Chiralpak AD-3 column with a mobile phase consisting of CO 2 and 0.2% cyclohexylamine in 2-propanol. The injection volume was 2 μL and run-time was 6 min. MS/MS detection was performed with positive electrospray ionization and two multiple reaction monitoring transitions (m/z 136.1 > 119.0 and m/z 136.1 > 91.0). The calibration range was 50-10,000 ng/mL for each enantiomer. The between-assay relative standard deviations were in the range of 3.7-7.6%. Recovery was 92-93% and matrix effects ranged from 100 to 104% corrected with internal standard. After development and validation, the method has been successfully implemented in routine use at our laboratory for both separation and quantification of R/S-amphetamine, and has proved to be a reliable and useful tool for distinguishing intake of R- and S-amphetamine in authentic patient samples. Copyright © 2018 Elsevier B.V. All rights reserved.

Simultaneous separation and determination of praeruptorin A, B and C by micellar electrokinetic chromatography using sodium dodecyl sulphate and sodium cholate as mixed micelles.

PubMed

Chen, Meng; Chang, Ruimiao; Xu, Liying; Huang, Yayun; Zhang, Hongfen; Chen, Anjia

2018-02-02

Praeruptorin A, B and C are major bioactive constituents in Peucedani Radix. They display anti-inflammatory effect, anti-hypertension effect, antiplatelet aggregation, potential anti-cancer activities and so on. They are worthy of investigation as potentially novel and versatile drugs. To develop a method using micellar electrokinetic chromatography (MEKC) for the application in simultaneously separation and determination of praeruptorin A, B and C from Peucedani Radix and its medicinal preparations. Method optimisation was carried out by investigating influences of significant factors on the separation. The method was subjected to validation. The determination of praeruptorin A, B and C in Peucedani Radix and its drug formulations was accomplished by the developed method. The optimal separation condition was 20 mM borate buffer containing 40 mM sodium cholate (SC), 22 mM sodium dodecyl sulphate (SDS) and 25% (v/v) acetonitrile (pH 10.00); 15 kV of voltage; 25°C of temperature; detection at 224 nm. Under this condition, three analytes were baseline separated within 16 min. A good linearity was obtained with correlation coefficients from 0.9988 to 0.9995. The limits of detection (LODs) and limits of quantitation (LOQs) ranged from 0.50 to 0.80 μg/mL and from 1.50 to 2.50 μg/mL, respectively. The recoveries ranged between 95.3% and 103.4%. The proposed method has been successfully applied to the simultaneous determination of praeruptorin A, B and C in Peucedani Radix and its pharmaceutical preparations. Additionally, it could be a potential alternative to the quality control of Peucedani Radix. Copyright © 2018 John Wiley & Sons, Ltd.

An adaptive toolbox approach to the route to expertise in sport.

PubMed

de Oliveira, Rita F; Lobinger, Babett H; Raab, Markus

2014-01-01

Expertise is characterized by fast decision-making which is highly adaptive to new situations. Here we propose that athletes use a toolbox of heuristics which they develop on their route to expertise. The development of heuristics occurs within the context of the athletes' natural abilities, past experiences, developed skills, and situational context, but does not pertain to any of these factors separately. This is a novel approach because it integrates separate factors into a comprehensive heuristic description. The novelty of this approach lies within the integration of separate factors determining expertise into a comprehensive heuristic description. It is our contention that talent identification methods and talent development models should therefore be geared toward the assessment and development of specific heuristics. Specifically, in addition to identifying and developing separate natural abilities and skills as per usual, heuristics should be identified and developed. The application of heuristics to talent and expertise models can bring the field one step away from dichotomized models of nature and nurture toward a comprehensive approach to the route to expertise.

An adaptive toolbox approach to the route to expertise in sport

PubMed Central

de Oliveira, Rita F.; Lobinger, Babett H.; Raab, Markus

2014-01-01

Expertise is characterized by fast decision-making which is highly adaptive to new situations. Here we propose that athletes use a toolbox of heuristics which they develop on their route to expertise. The development of heuristics occurs within the context of the athletes’ natural abilities, past experiences, developed skills, and situational context, but does not pertain to any of these factors separately. This is a novel approach because it integrates separate factors into a comprehensive heuristic description. The novelty of this approach lies within the integration of separate factors determining expertise into a comprehensive heuristic description. It is our contention that talent identification methods and talent development models should therefore be geared toward the assessment and development of specific heuristics. Specifically, in addition to identifying and developing separate natural abilities and skills as per usual, heuristics should be identified and developed. The application of heuristics to talent and expertise models can bring the field one step away from dichotomized models of nature and nurture toward a comprehensive approach to the route to expertise. PMID:25071673

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wu, Chaochao; Duan, Jicheng; Liu, Tao

Human biofluids, especially blood plasma or serum, hold great potential as the sources of candidate biomarkers for various diseases; however, the enormous dynamic range of protein concentrations in biofluids represents a significant analytical challenge for detecting promising low-abundance proteins. Over the last decade, various immunoaffinity chromatographic methods have been developed and routinely applied for separating low-abundance proteins from the high- and moderate-abundance proteins, thus enabling much more effective detection of low-abundance proteins. Herein, we review the advances of immunoaffinity separation methods and their contributions to the proteomic applications in human biofluids. The limitations and future perspectives of immunoaffinity separation methodsmore » are also discussed.« less

Analysis of benzo(a)pyrene in airborne particulates by gas chromatography

NASA Technical Reports Server (NTRS)

Luedecke, E.

1976-01-01

A routine method was developed to measure benzo(a)pyrene in airborne particulates. Samples were collected on a filter and the organic portion was extracted with cyclohexane. The polynuclear hydrocarbon (PNHC) fraction was separated from the aliphatics by column chromatography. An internal standard was added to the extract and a portion of it was injected into a gas chromatograph. Although the gas chromatographic method has often been reported in the literature, satisfactory separation of benzo(a)pyrene and benzo(e)pyrene has not been achieved. With the introduction of a nematic liquid crystal as the stationary phase good separation is now possible.

Rapid, economical qualitative method for separation of aflatoxins B-1, B-2 & G-1, G-2 by dry column chromatography.

PubMed

Megalla, S E

1983-12-01

A good correlation of four components of aflatoxins was accomplished by using the dry column chromatography method. The decolorization process of interfering substances, by 0.01 N KOH and defatting the extract with petroleum ether yields a clean residue for DCC separation. It is clear that the dry column chromatography is a very simple and time-saving procedure for separation of aflatoxins. DCC columns are more economical than precoated 'thick layer' preparative plates and, in DCC, no large developing tanks need to be used. Hazards associated with the use of large volumes of flammable solvents are greatly reduced.

Introducing 3D U-statistic method for separating anomaly from background in exploration geochemical data with associated software development

NASA Astrophysics Data System (ADS)

Ghannadpour, Seyyed Saeed; Hezarkhani, Ardeshir

2016-03-01

The U-statistic method is one of the most important structural methods to separate the anomaly from the background. It considers the location of samples and carries out the statistical analysis of the data without judging from a geochemical point of view and tries to separate subpopulations and determine anomalous areas. In the present study, to use U-statistic method in three-dimensional (3D) condition, U-statistic is applied on the grade of two ideal test examples, by considering sample Z values (elevation). So far, this is the first time that this method has been applied on a 3D condition. To evaluate the performance of 3D U-statistic method and in order to compare U-statistic with one non-structural method, the method of threshold assessment based on median and standard deviation (MSD method) is applied on the two example tests. Results show that the samples indicated by U-statistic method as anomalous are more regular and involve less dispersion than those indicated by the MSD method. So that, according to the location of anomalous samples, denser areas of them can be determined as promising zones. Moreover, results show that at a threshold of U = 0, the total error of misclassification for U-statistic method is much smaller than the total error of criteria of bar {x}+n× s. Finally, 3D model of two test examples for separating anomaly from background using 3D U-statistic method is provided. The source code for a software program, which was developed in the MATLAB programming language in order to perform the calculations of the 3D U-spatial statistic method, is additionally provided. This software is compatible with all the geochemical varieties and can be used in similar exploration projects.

A Self-Directed Method for Cell-Type Identification and Separation of Gene Expression Microarrays

PubMed Central

Zuckerman, Neta S.; Noam, Yair; Goldsmith, Andrea J.; Lee, Peter P.

2013-01-01

Gene expression analysis is generally performed on heterogeneous tissue samples consisting of multiple cell types. Current methods developed to separate heterogeneous gene expression rely on prior knowledge of the cell-type composition and/or signatures - these are not available in most public datasets. We present a novel method to identify the cell-type composition, signatures and proportions per sample without need for a-priori information. The method was successfully tested on controlled and semi-controlled datasets and performed as accurately as current methods that do require additional information. As such, this method enables the analysis of cell-type specific gene expression using existing large pools of publically available microarray datasets. PMID:23990767

MULTIPOLLUTANT METHODS - METHODS FOR OZONE AND OZONE PRECURSORS

EPA Science Inventory

This task involves the development and testing of methods for monitoring ozone and compounds associated with the atmospheric chemistry of ozone production both as precursors and reaction products. Although atmospheric gases are the primary interest, separation of gas and particl...

Ion exchange separation of chromium from natural water matrix for stable isotope mass spectrometric analysis

USGS Publications Warehouse

Ball, J.W.; Bassett, R.L.

2000-01-01

A method has been developed for separating the Cr dissolved in natural water from matrix elements and determination of its stable isotope ratios using solid-source thermal-ionization mass spectrometry (TIMS). The separation method takes advantage of the existence of the oxidized form of Cr as an oxyanion to separate it from interfering cations using anion-exchange chromatography, and of the reduced form of Cr as a positively charged ion to separate it from interfering anions such as sulfate. Subsequent processing of the separated sample eliminates residual organic material for application to a solid source filament. Ratios for 53Cr/52Cr for National Institute of Standards and Technology Standard Reference Material 979 can be measured using the silica gel-boric acid technique with a filament-to-filament standard deviation in the mean 53Cr/52Cr ratio for 50 replicates of 0.00005 or less. (C) 2000 Elsevier Science B.V. All rights reserved.

Nonaqueous capillary electrophoresis of dextromethorphan and its metabolites.

PubMed

Pelcová, Marta; Langmajerová, Monika; Cvingráfová, Eliška; Juřica, Jan; Glatz, Zdeněk

2014-10-01

This study deals with the nonaqueous capillary electrophoretic separation of dextromethorphan and its metabolites using a methanolic background electrolyte. The optimization of separation conditions was performed in terms of the resolution of dextromethorphan and dextrorphan and the effect of separation temperature, voltage, and the characteristics of the background electrolyte were studied. Complete separation of all analytes was achieved in 40 mM ammonium acetate dissolved in methanol. Hydrodynamic injection was performed at 3 kPa for 4 s. The separation voltage was 20 kV accompanied by a low electric current. The ultraviolet detection was performed at 214 nm, the temperature of the capillary was 25°C. These conditions enabled the separation of four analytes plus the internal standard within 9 min. Further, the developed method was validated in terms of linearity, sensitivity, and repeatability. Rat liver perfusate samples were subjected to the nonaqueous capillary electrophoretic method to illustrate its applicability. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Separation of nuclear isomers for cancer therapeutic radionuclides based on nuclear decay after-effects.

PubMed

Bhardwaj, R; van der Meer, A; Das, S K; de Bruin, M; Gascon, J; Wolterbeek, H T; Denkova, A G; Serra-Crespo, P

2017-03-13

177 Lu has sprung as a promising radionuclide for targeted therapy. The low soft tissue penetration of its β - emission results in very efficient energy deposition in small-size tumours. Because of this, 177 Lu is used in the treatment of neuroendocrine tumours and is also clinically approved for prostate cancer therapy. In this work, we report a separation method that achieves the challenging separation of the physically and chemically identical nuclear isomers, 177m Lu and 177 Lu. The separation method combines the nuclear after-effects of the nuclear decay, the use of a very stable chemical complex and a chromatographic separation. Based on this separation concept, a new type of radionuclide generator has been devised, in which the parent and the daughter radionuclides are the same elements. The 177m Lu/ 177 Lu radionuclide generator provides a new production route for the therapeutic radionuclide 177 Lu and can bring significant growth in the research and development of 177 Lu based pharmaceuticals.

Separation of left and right lungs using 3-dimensional information of sequential computed tomography images and a guided dynamic programming algorithm.

PubMed

Park, Sang Cheol; Leader, Joseph Ken; Tan, Jun; Lee, Guee Sang; Kim, Soo Hyung; Na, In Seop; Zheng, Bin

2011-01-01

This article presents a new computerized scheme that aims to accurately and robustly separate left and right lungs on computed tomography (CT) examinations. We developed and tested a method to separate the left and right lungs using sequential CT information and a guided dynamic programming algorithm using adaptively and automatically selected start point and end point with especially severe and multiple connections. The scheme successfully identified and separated all 827 connections on the total 4034 CT images in an independent testing data set of CT examinations. The proposed scheme separated multiple connections regardless of their locations, and the guided dynamic programming algorithm reduced the computation time to approximately 4.6% in comparison with the traditional dynamic programming and avoided the permeation of the separation boundary into normal lung tissue. The proposed method is able to robustly and accurately disconnect all connections between left and right lungs, and the guided dynamic programming algorithm is able to remove redundant processing.

A fast and sensitive method for the separation of carotenoids using ultra-high performance supercritical fluid chromatography-mass spectrometry.

PubMed

Jumaah, Firas; Plaza, Merichel; Abrahamsson, Victor; Turner, Charlotta; Sandahl, Margareta

2016-08-01

In this study, a rapid and sensitive ultra-high performance supercritical fluid chromatography-mass spectrometry (UHPSFC-MS) method has been developed and partially validated for the separation of carotenoids within less than 6 min. Six columns of orthogonal selectivity were examined, and the best separation was obtained by using a 1-aminoanthracene (1-AA) column. The length of polyene chain as well as the number of hydroxyl groups in the structure of the studied carotenoids determines their differences in the physiochemical properties and thus the separation that is achieved on this column. All of the investigated carotenoids were baseline separated with resolution values greater than 1.5. The effects of gradient program, back pressure, and column temperature were studied with respect to chromatographic properties such as retention and selectivity. Electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI) were compared in both positive and negative mode, using both direct infusion and hyphenated with UHPSFC. The ESI in positive mode provided the highest response. The coefficient of determination (R (2)) for all calibration curves were greater than 0.998. Limit of detection (LOD) was in the range of 2.6 and 25.2 ng/mL for α-carotene and astaxanthin, respectively, whereas limit of quantification (LOQ) was in the range of 7.8 and 58.0 ng/mL for α-carotene and astaxanthin, respectively. Repeatability and intermediate precision of the developed UHPSFC-MS method were determined and found to be RSD < 3 % and RSD < 6 %, respectively. The method was applied in order to determine carotenoids in supercritical fluid extracts of microalgae and rosehip. Graphical Abstract Ultra-high performance supercritical fluid chromatography-a rapid separation method for the analysis of carotenoids in rosehip and microalgae samples.

Acoustic separation of circulating tumor cells

PubMed Central

Li, Peng; Mao, Zhangming; Peng, Zhangli; Zhou, Lanlan; Chen, Yuchao; Huang, Po-Hsun; Truica, Cristina I.; Drabick, Joseph J.; El-Deiry, Wafik S.; Dao, Ming; Suresh, Subra; Huang, Tony Jun

2015-01-01

Circulating tumor cells (CTCs) are important targets for cancer biology studies. To further elucidate the role of CTCs in cancer metastasis and prognosis, effective methods for isolating extremely rare tumor cells from peripheral blood must be developed. Acoustic-based methods, which are known to preserve the integrity, functionality, and viability of biological cells using label-free and contact-free sorting, have thus far not been successfully developed to isolate rare CTCs using clinical samples from cancer patients owing to technical constraints, insufficient throughput, and lack of long-term device stability. In this work, we demonstrate the development of an acoustic-based microfluidic device that is capable of high-throughput separation of CTCs from peripheral blood samples obtained from cancer patients. Our method uses tilted-angle standing surface acoustic waves. Parametric numerical simulations were performed to design optimum device geometry, tilt angle, and cell throughput that is more than 20 times higher than previously possible for such devices. We first validated the capability of this device by successfully separating low concentrations (∼100 cells/mL) of a variety of cancer cells from cell culture lines from WBCs with a recovery rate better than 83%. We then demonstrated the isolation of CTCs in blood samples obtained from patients with breast cancer. Our acoustic-based separation method thus offers the potential to serve as an invaluable supplemental tool in cancer research, diagnostics, drug efficacy assessment, and therapeutics owing to its excellent biocompatibility, simple design, and label-free automated operation while offering the capability to isolate rare CTCs in a viable state. PMID:25848039

Acoustic separation of circulating tumor cells.

PubMed

Li, Peng; Mao, Zhangming; Peng, Zhangli; Zhou, Lanlan; Chen, Yuchao; Huang, Po-Hsun; Truica, Cristina I; Drabick, Joseph J; El-Deiry, Wafik S; Dao, Ming; Suresh, Subra; Huang, Tony Jun

2015-04-21

Circulating tumor cells (CTCs) are important targets for cancer biology studies. To further elucidate the role of CTCs in cancer metastasis and prognosis, effective methods for isolating extremely rare tumor cells from peripheral blood must be developed. Acoustic-based methods, which are known to preserve the integrity, functionality, and viability of biological cells using label-free and contact-free sorting, have thus far not been successfully developed to isolate rare CTCs using clinical samples from cancer patients owing to technical constraints, insufficient throughput, and lack of long-term device stability. In this work, we demonstrate the development of an acoustic-based microfluidic device that is capable of high-throughput separation of CTCs from peripheral blood samples obtained from cancer patients. Our method uses tilted-angle standing surface acoustic waves. Parametric numerical simulations were performed to design optimum device geometry, tilt angle, and cell throughput that is more than 20 times higher than previously possible for such devices. We first validated the capability of this device by successfully separating low concentrations (∼100 cells/mL) of a variety of cancer cells from cell culture lines from WBCs with a recovery rate better than 83%. We then demonstrated the isolation of CTCs in blood samples obtained from patients with breast cancer. Our acoustic-based separation method thus offers the potential to serve as an invaluable supplemental tool in cancer research, diagnostics, drug efficacy assessment, and therapeutics owing to its excellent biocompatibility, simple design, and label-free automated operation while offering the capability to isolate rare CTCs in a viable state.

Simultaneous Separation of Actinium and Radium Isotopes from a Proton Irradiated Thorium Matrix

DOE PAGES

Mastren, Tara; Radchenko, Valery; Owens, Allison; ...

2017-08-15

A new method has been developed for the isolation of 223,224,225Ra, in high yield and purity, from a proton irradiated 232Th matrix. We report an all-aqueous process using multiple solid-supported adsorption steps including a citrate chelation method developed to remove >99.9% of the barium contaminants by activity from the final radium product. Moreover, we developed a procedure involving the use of three columns in succession, and the separation of 223,224,225Ra from the thorium matrix was obtained with an overall recovery yield of 91 ± 3%, average radiochemical purity of 99.9%, and production yields that correspond to physical yields based onmore » previously measured excitation functions.« less

Recent development in liquid chromatography stationary phases for separation of Traditional Chinese Medicine components.

PubMed

Jin, Hongli; Liu, Yanfang; Guo, Zhimou; Wang, Jixia; Zhang, Xiuli; Wang, Chaoran; Liang, Xinmiao

2016-10-25

Traditional Chinese Medicine (TCM) is an ancient medical practice which has been used to prevent and cure diseases for thousands of years. TCMs are frequently multi-component systems with mainly unidentified constituents. The study of the chemical compositions of TCMs remains a hotspot of research. Different strategies have been developed to manage the significant complexity of TCMs, in an attempt to determine their constituents. Reversed-phase liquid chromatography (RPLC) is still the method of choice for the separation of TCMs, but has many problems related to limited selectivity. Recently, enormous efforts have been concentrated on the development of efficient liquid chromatography (LC) methods for TCMs, based on selective stationary phases. This can improve the resolution and peak capacity considerably. In addition, high-efficiency stationary phases have been applied in the analysis of TCMs since the invention of ultra high-performance liquid chromatography (UHPLC). This review describes the advances in LC methods in TCM research from 2010 to date, and focuses on novel stationary phases. Their potential in the separation of TCMs using relevant applications is also demonstrated. Copyright © 2016 Elsevier B.V. All rights reserved.

Development, validation and evaluation of an analytical method for the determination of monomeric and oligomeric procyanidins in apple extracts.

PubMed

Hollands, Wendy J; Voorspoels, Stefan; Jacobs, Griet; Aaby, Kjersti; Meisland, Ane; Garcia-Villalba, Rocio; Tomas-Barberan, Francisco; Piskula, Mariusz K; Mawson, Deborah; Vovk, Irena; Needs, Paul W; Kroon, Paul A

2017-04-28

There is a lack of data for individual oligomeric procyanidins in apples and apple extracts. Our aim was to develop, validate and evaluate an analytical method for the separation, identification and quantification of monomeric and oligomeric flavanols in apple extracts. To achieve this, we prepared two types of flavanol extracts from freeze-dried apples; one was an epicatechin-rich extract containing ∼30% (w/w) monomeric (-)-epicatechin which also contained oligomeric procyanidins (Extract A), the second was an oligomeric procyanidin-rich extract depleted of epicatechin (Extract B). The parameters considered for method optimisation were HPLC columns and conditions, sample heating, mass of extract and dilution volumes. The performance characteristics considered for method validation included standard linearity, method sensitivity, precision and trueness. Eight laboratories participated in the method evaluation. Chromatographic separation of the analytes was best achieved utilizing a Hilic column with a binary mobile phase consisting of acidic acetonitrile and acidic aqueous methanol. The final method showed linearity for epicatechin in the range 5-100μg/mL with a correlation co-efficient >0.999. Intra-day and inter-day precision of the analytes ranged from 2 to 6% and 2 to 13% respectively. Up to dp3, trueness of the method was >95% but decreased with increasing dp. Within laboratory precision showed RSD values <5 and 10% for monomers and oligomers, respectively. Between laboratory precision was 4 and 15% (Extract A) and 7 and 30% (Extract B) for monomers and oligomers, respectively. An analytical method for the separation, identification and quantification of procyanidins in an apple extract was developed, validated and assessed. The results of the inter-laboratory evaluation indicate that the method is reliable and reproducible. Copyright © 2017. Published by Elsevier B.V.

Single Wall Nanotube Type-Specific Functionalization and Separation

NASA Technical Reports Server (NTRS)

Boul, Peter; Nikolaev, Pavel; Sosa, Edward; Arepalli, Sivaram; Yowell, Leonard

2008-01-01

Metallic single-wall carbon nanotubes were selectively solubilized in THF and separated from semiconducting nanotubes. Once separated, the functionalized metallic tubes were de-functionalized to restore their metallic band structure. Absorption and Raman spectroscopy of the enriched samples support conclusions of the enrichment of nanotube samples by metallic type. A scalable method for enriching nanotube conductive type has been developed. Raman and UV-Vis data indicate SWCNT reaction with dodecylbenzenediazonium results in metallic enrichment. It is expected that further refinement of this techniques will lead to more dramatic separations of types and diameters.

Chemical separation of Nd from geological samples for chronological studies using (146)Sm-(142)Nd and (147)Sm-(143)Nd systematics.

PubMed

Kagami, Saya; Yokoyama, Tetsuya

2016-09-21

Sm-Nd dating, which involves long-lived (147)Sm-(143)Nd and short-lived (146)Sm-(142)Nd systematics, has been widely used in the field of geosciences. To obtain precise and accurate ages of geological samples, the determination of highly precise Nd isotope ratios with nearly complete removal of Ce and Sm is indispensable to avoid mass spectral interference. In this study, we developed a three-step column chemistry procedure for separating Nd from geological samples that includes cation exchange chromatography for separating major elements from rare earth elements (REEs), oxidative extraction chromatography using Ln Resin coupled with HNO3 + KBrO3 for separating tetravalent Ce from the remaining REEs, and final purification of Nd using Ln Resin. This method enables high recovery of Nd (>91%) with effective separation of Nd from Ce and Sm (Ce/Nd < 1.2 × 10(-5) and Sm/Nd < 5.2 × 10(-6)). In addition, we devised a new method for determining Sm/Nd ratios with the isotope dilution inductively coupled plasma mass spectrometry method using (145)Nd- and (149)Sm-enriched spikes coupled with a group separation of REEs using TRU Resin. Applying the techniques developed in this study, we determined the Sm-Nd whole-rock isochron age of basaltic eucrites, yielding 4577 - 88(+ 55) Ma and 4558 ± 300 Ma for (146)Sm-(142)Nd and (147)Sm-(143)Nd systematics, respectively. Copyright © 2016 Elsevier B.V. All rights reserved.

Connection method of separated luminal regions of intestine from CT volumes

NASA Astrophysics Data System (ADS)

Oda, Masahiro; Kitasaka, Takayuki; Furukawa, Kazuhiro; Watanabe, Osamu; Ando, Takafumi; Hirooka, Yoshiki; Goto, Hidemi; Mori, Kensaku

2015-03-01

This paper proposes a connection method of separated luminal regions of the intestine for Crohn's disease diagnosis. Crohn's disease is an inflammatory disease of the digestive tract. Capsule or conventional endoscopic diagnosis is performed for Crohn's disease diagnosis. However, parts of the intestines may not be observed in the endoscopic diagnosis if intestinal stenosis occurs. Endoscopes cannot pass through the stenosed parts. CT image-based diagnosis is developed as an alternative choice of the Crohn's disease. CT image-based diagnosis enables physicians to observe the entire intestines even if stenosed parts exist. CAD systems for Crohn's disease using CT volumes are recently developed. Such CAD systems need to reconstruct separated luminal regions of the intestines to analyze intestines. We propose a connection method of separated luminal regions of the intestines segmented from CT volumes. The luminal regions of the intestines are segmented from a CT volume. The centerlines of the luminal regions are calculated by using a thinning process. We enumerate all the possible sequences of the centerline segments. In this work, we newly introduce a condition using distance between connected ends points of the centerline segments. This condition eliminates unnatural connections of the centerline segments. Also, this condition reduces processing time. After generating a sequence list of the centerline segments, the correct sequence is obtained by using an evaluation function. We connect the luminal regions based on the correct sequence. Our experiments using four CT volumes showed that our method connected 6.5 out of 8.0 centerline segments per case. Processing times of the proposed method were reduced from the previous method.

Microchannel gel electrophoretic separation systems and methods for preparing and using

DOEpatents

Herr, Amy E; Singh, Anup K; Throckmorton, Daniel J

2015-02-24

A micro-analytical platform for performing electrophoresis-based immunoassays was developed by integrating photopolymerized cross-linked polyacrylamide gels within a microfluidic device. The microfluidic immunoassays are performed by gel electrophoretic separation and quantifying analyte concentration based upon conventional polyacrylamide gel electrophoresis (PAGE). To retain biological activity of proteins and maintain intact immune complexes, native PAGE conditions were employed. Both direct (non-competitive) and competitive immunoassay formats are demonstrated in microchips for detecting toxins and biomarkers (cytokines, c-reactive protein) in bodily fluids (serum, saliva, oral fluids). Further, a description of gradient gels fabrication is included, in an effort to describe methods we have developed for further optimization of on-chip PAGE immunoassays. The described chip-based PAGE immunoassay method enables immunoassays that are fast (minutes) and require very small amounts of sample (less than a few microliters). Use of microfabricated chips as a platform enables integration, parallel assays, automation and development of portable devices.

Microchannel gel electrophoretic separation systems and methods for preparing and using

DOEpatents

Herr, Amy; Singh, Anup K; Throckmorton, Daniel J

2013-09-03

A micro-analytical platform for performing electrophoresis-based immunoassays was developed by integrating photopolymerized cross-linked polyacrylamide gels within a microfluidic device. The microfluidic immunoassays are performed by gel electrophoretic separation and quantifying analyte concentration based upon conventional polyacrylamide gel electrophoresis (PAGE). To retain biological activity of proteins and maintain intact immune complexes, native PAGE conditions were employed. Both direct (non-competitive) and competitive immunoassay formats are demonstrated in microchips for detecting toxins and biomarkers (cytokines, c-reactive protein) in bodily fluids (serum, saliva, oral fluids). Further, a description of gradient gels fabrication is included, in an effort to describe methods we have developed for further optimization of on-chip PAGE immunoassays. The described chip-based PAGE immunoassay method enables immunoassays that are fast (minutes) and require very small amounts of sample (less than a few microliters). Use of microfabricated chips as a platform enables integration, parallel assays, automation and development of portable devices.

Rapid fusion method for the determination of Pu, Np, and Am in large soil samples

DOE PAGES

Maxwell, Sherrod L.; Culligan, Brian; Hutchison, Jay B.; ...

2015-02-14

A new rapid sodium hydroxide fusion method for the preparation of 10-20 g soil samples has been developed by the Savannah River National Laboratory (SRNL). The method enables lower detection limits for plutonium, neptunium, and americium in environmental soil samples. The method also significantly reduces sample processing time and acid fume generation compared to traditional soil digestion techniques using hydrofluoric acid. Ten gram soil aliquots can be ashed and fused using the new method in 1-2 hours, completely dissolving samples, including refractory particles. Pu, Np and Am are separated using stacked 2mL cartridges of TEVA and DGA Resin and measuredmore » using alpha spectrometry. The method can be adapted for measurement by inductively-coupled plasma mass spectrometry (ICP-MS). Two 10 g soil aliquots of fused soil may be combined prior to chromatographic separations to further improve detection limits. Total sample preparation time, including chromatographic separations and alpha spectrometry source preparation, is less than 8 hours.« less

A simple method for the investigation of cell separation effects of blood with physiological hematocrit values.

PubMed

Gester, Kathrin; Jansen, Sebastian V; Stahl, Marion; Steinseifer, Ulrich

2015-05-01

Even though the separation of blood into erythrocyte-rich and erythrocyte-poor areas is well known in physiological setups such as small vessels, it has recently come into focus in small gaps in cardiovascular applications. Studies show that separation effects occur, for example, in gaps in hydrodynamic bearings, where they can have a positive effect on hemolysis. Separation effects depend on the hematocrit value, but due to visualization issues, studies in small gaps used very low hematocrit values. In this study, a test setup and an evaluation method for the investigation of separation effects of blood with hematocrit values of 30, 45, and 60% were developed. The erythrocyte distribution was evaluated by means of gray scale value distribution. This principle is based on the fact that an erythrocyte-rich region is more opaque than an erythrocyte-poor region. The experimental setup is designed in a way that no further processes (e.g., fluorescence labeling) need to be carried out which might change the properties of the membrane of the erythrocytes, and therefore their flow properties. Additionally, the method is executable with basic laboratory equipment, which makes it applicable for many laboratories. To validate the feasibility of the method, the influence of the diameter and the flow rate on the migration of erythrocytes were studied in micro channels for three different physiological hematocrit values. Even though no individual cells were traced, plasma layer and areas of high erythrocyte concentration could be identified. Dependencies of the erythrocyte distribution on flow rate and channel diameter were validated. The influence of the hematocrit value was demonstrated as well and showed the hematocrit value to be a crucial factor when investigating cell separation. The experimental results were consistent with findings in the literature. As the developed method is suitable for physiological hematocrit values and easy to handle, it provides an optimal basis for cell separation studies in gap models with whole blood, for example, hydrodynamic bearings, where it can be used to optimize these devices. Copyright © 2014 International Center for Artificial Organs and Transplantation and Wiley Periodicals, Inc.

Orbiter Repair Maneuver Contingency Separation Methods and Analysis

NASA Technical Reports Server (NTRS)

Machula, Michael

2005-01-01

Repairing damaged thermal protection system tile requires the Space Shuttle to be oriented such that repair platform access from the International Space Station (ISS) is possible. To do this, the Space Shuttle uses the Orbiter Repair Maneuver (ORM), which utilizes the Shuttle Remote Manipulator System (SRMS) to rotate the Space Shuttle in relation to the ISS, for extended periods of time. These positions cause difficulties and challenges to performing a safe separation (no collision or thruster plume damage to sensitive ISS structures) should an inadvertent release occur or a contingency procedure require it. To help protect for an SRMS failure or other failures, a method for separating without collision and the ability to redock to ISS from the ORM configuration was needed. The contingency ORM separation solution elegantly takes advantage of orbital mechanics between ISS and the separating Space Shuttle. By pitching the ISS down approximately 45 degrees, in a majority of the ORM repair positions, the altitude difference between the ISS and Space Shuttle center of gravity is maximized. This altitude difference results in different orbital energies (orbital periods) causing objects to separate from each other without requiring translational firings. Using this method, a safe contingency ORM separation is made possible in many odd positions even though some separation positions point high powered thrusters directly at fragile ISS and Soyuz solar arrays. Documented in this paper are the development simulations and procedures of the contingency ORM separation and the challenges encountered with large constraints to work around. Lastly, a method of returning to redock with the ISS to pick up the stranded crew members (or transfer the final crew members) is explained as well as the thruster and ISS loads analysis.

PHYSICAL BENEFICATION OF LOW-GRADE URANIUM ORES

DOE Office of Scientific and Technical Information (OSTI.GOV)

Butler, J.N.

1958-07-30

Investigations are presented of methods for the physi cal beneficiation of low-grade and other uranium ores. The investlgations which have been in progress since September 1952 cover work done on a variety of natural ores, as well as a certain amount of basic research on mixtures of synthetic or high-grade natural uranium minerais with various gangues. Methods of beneficlation investigated include flotation, wet and dry attroftioning, magnetic separation. electresiatie separation, and misceilaneous minor methods. A rapid, routine method oicolorimeiric determlnation of uranium was also developed in order to facilitaie analyzing of low-grade materials for uranium. This proeedure is presenied inmore » condensed form. (auth)« less

Assessment of Entrepreneurial Territorial Attractiveness by the Ranking Method

ERIC Educational Resources Information Center

Gavrilova, Marina A.; Shepelev, Victor M.; Kosyakova, Inessa V.; Belikova, Lyudmila F.; Chistik, Olga F.

2016-01-01

The relevance of the researched problem is caused by existence of differentiation in development of separate regional units (urban districts and municipalities) within the region. The aim of this article is to offer a method, which determines the level of differentiation in development of various components of the region, and also in producing a…

COMPUTER-ASSISTED HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD DEVELOPMENT WITH APPLICATIONS TO THE ISOLATION AND ANALYSIS OF PHYTOPLANKTON PIGMENTS. (R826944)

EPA Science Inventory

We used chromatography modeling software to assist in HPLC method development, with the goal
of enhancing separations through the exclusive use of gradient time and column temperature. We
surveyed nine stationary phases for their utility in pigment purification and natur...

Determining Aqueous Fullerene Particle Size Distributions by Asymmetric Flow Field-Flow Fractionation (AF4) without Surfactants

EPA Science Inventory

To determine the behavior of nanoparticles in environmental systems, methods must be developed to measure nanoparticle size. Asymmetric Flow Field Flow Fractionation (AF4) is an aqueous compatible size separation technique which is able to separate particles from 1 nm to 10 µm in...

Optimization of tomato pomace separation using air aspirator system by response surface methodology

USDA-ARS?s Scientific Manuscript database

Tomato pomace contains seeds and peels which are rich in protein and fat, and dietary fiber and lycopene, respectively. It is important to develop a suitable method to separate seeds and peel in tomato pomace for achieving value-added utilization of tomato pomace. The objectives of this research wer...

Separation and purification of both tea seed polysaccharide and saponin from camellia cake extract using macroporous resin.

PubMed

Yang, Pengjie; Zhou, Mingda; Zhou, Chengyun; Wang, Qian; Zhang, Fangfang; Chen, Jian

2015-02-01

A novel method to separate and purify tea seed polysaccharide and tea seed saponin from camellia cake extract by macroporous resin was developed. Among four kinds of resins (AB-8, NKA-9, XDA-6, and D4020) tested, AB-8 macroporous resin possessed optimal separating capacity for the two substances and thus was selected for the separation, in which deionized water was used to elute tea seed polysaccharide, 0.25% NaOH solution to remove the undesired pigments, and 90% ethanol to elute tea seed saponin. Further dynamic adsorption/desorption experiments on AB-8 resin-based column chromatography were conducted to obtain the optimal parameters. Under optimal dynamic adsorption and desorption conditions, 18.7 and 11.8% yield of tea seed polysaccharide and tea seed saponin were obtained with purities of 89.2 and 96.0%, respectively. The developed method provides a potential approach for the large-scale production of tea seed polysaccharide and tea seed saponin from camellia cake. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Analysis of spatial heterogeneity in normal epithelium and preneoplastic alterations in mouse prostate tumor models

PubMed Central

Valkonen, Mira; Ruusuvuori, Pekka; Kartasalo, Kimmo; Nykter, Matti; Visakorpi, Tapio; Latonen, Leena

2017-01-01

Cancer involves histological changes in tissue, which is of primary importance in pathological diagnosis and research. Automated histological analysis requires ability to computationally separate pathological alterations from normal tissue with all its variables. On the other hand, understanding connections between genetic alterations and histological attributes requires development of enhanced analysis methods suitable also for small sample sizes. Here, we set out to develop computational methods for early detection and distinction of prostate cancer-related pathological alterations. We use analysis of features from HE stained histological images of normal mouse prostate epithelium, distinguishing the descriptors for variability between ventral, lateral, and dorsal lobes. In addition, we use two common prostate cancer models, Hi-Myc and Pten+/− mice, to build a feature-based machine learning model separating the early pathological lesions provoked by these genetic alterations. This work offers a set of computational methods for separation of early neoplastic lesions in the prostates of model mice, and provides proof-of-principle for linking specific tumor genotypes to quantitative histological characteristics. The results obtained show that separation between different spatial locations within the organ, as well as classification between histologies linked to different genetic backgrounds, can be performed with very high specificity and sensitivity. PMID:28317907

Method optimization for drug impurity profiling in supercritical fluid chromatography: Application to a pharmaceutical mixture.

PubMed

Muscat Galea, Charlene; Didion, David; Clicq, David; Mangelings, Debby; Vander Heyden, Yvan

2017-12-01

A supercritical chromatographic method for the separation of a drug and its impurities has been developed and optimized applying an experimental design approach and chromatogram simulations. Stationary phase screening was followed by optimization of the modifier and injection solvent composition. A design-of-experiment (DoE) approach was then used to optimize column temperature, back-pressure and the gradient slope simultaneously. Regression models for the retention times and peak widths of all mixture components were built. The factor levels for different grid points were then used to predict the retention times and peak widths of the mixture components using the regression models and the best separation for the worst separated peak pair in the experimental domain was identified. A plot of the minimal resolutions was used to help identifying the factor levels leading to the highest resolution between consecutive peaks. The effects of the DoE factors were visualized in a way that is familiar to the analytical chemist, i.e. by simulating the resulting chromatogram. The mixture of an active ingredient and seven impurities was separated in less than eight minutes. The approach discussed in this paper demonstrates how SFC methods can be developed and optimized efficiently using simple concepts and tools. Copyright © 2017 Elsevier B.V. All rights reserved.

Validation of an ultra-fast UPLC-UV method for the separation of antituberculosis tablets.

PubMed

Nguyen, Dao T-T; Guillarme, Davy; Rudaz, Serge; Veuthey, Jean-Luc

2008-04-01

A simple method using ultra performance LC (UPLC) coupled with UV detection was developed and validated for the determination of antituberculosis drugs in combined dosage form, i. e. isoniazid (ISN), pyrazinamide (PYR) and rifampicin (RIF). Drugs were separated on a short column (2.1 mm x 50 mm) packed with 1.7 mum particles, using an elution gradient procedure. At 30 degrees C, less than 2 min was necessary for the complete separation of the three antituberculosis drugs, while the original USP method was performed in 15 min. Further improvements were obtained with the combination of UPLC and high temperature (up to 90 degrees C), namely HT-UPLC, which allows the application of higher mobile phase flow rates. Therefore, the separation of ISN, PYR and RIF was performed in less than 1 min. After validation (selectivity, trueness, precision and accuracy), both methods (UPLC and HT-UPLC) have proven suitable for the routine quality control analysis of antituberculosis drugs in combined dosage form. Additionally, a large number of samples per day can be analysed due to the short analysis times.

Separated flow over bodies of revolution using an unsteady discrete-vorticity cross wake. Part 2: Computer program description

NASA Technical Reports Server (NTRS)

Marshall, F. J.; Deffenbaugh, F. D.

1974-01-01

A method is developed to determine the flow field of a body of revolution in separated flow. The computer was used to integrate various solutions and solution properties of the sub-flow fields which made up the entire flow field without resorting to a finite difference solution to the complete Navier-Stokes equations. The technique entails the use of the unsteady cross flow analogy and a new solution to the two-dimensional unsteady separated flow problem based upon an unsteady, discrete-vorticity wake. Data for the forces and moments on aerodynamic bodies at low speeds and high angle of attack (outside the range of linear inviscid theories) such that the flow is substantially separated are produced which compare well with experimental data. In addition, three dimensional steady separated regions and wake vortex patterns are determined. The computer program developed to perform the numerical calculations is described.

Vibration-type particle separation device with piezoceramic vibrator

NASA Astrophysics Data System (ADS)

Ooe, Katsutoshi; Doi, Akihiro

2008-12-01

During hemanalysis, it is necessary to separate blood cells from whole blood. Many blood separation methods, for example, centrifugation and filtering, are in practical use. However, the use of these methods involves problems from the perspectives of processing speed and processing volume. We develop new types of blood separation devices that use piezo-ceramic vibrators. The first device uses a capillary. One end of the capillary is fixed to the device frame, and the other is fixed to a piezo-ceramic vibrator. The vibrator transmits bending waves to the capillary. This device can process only a small amount of solution; therefore, it is not suitable for hemanalysis. In order to solve this problem, we developed a second device; this device has a pair of thin glass plates with a small gap as a substitute for the capillary used in the first device. These devices are based on the fact that particles heavier than water move toward transverse velocity antinodes while those lighter than water move toward velocity nodes. In this report, we demonstrate the highspeed separation of silica microbeads and 50-vol% glycerol water by using these devices. The first device can separate the abovementioned solution within 3 min while the second can separate it within 1 min. Both devices are driven by a rectangular wave of 15 to 20 Vpp. Furthermore, it has been confirmed that red blood cells are separated from diluted whole blood using the first device within approximately 1 min. These devices have transparency, so they can compose as the analysis system with the chemical analyzer easily.

Study for identification of beneficial uses of Space (BUS). Volume 2: Technical report. Book 1: Development and business analysis of space processed isoenzymes

NASA Technical Reports Server (NTRS)

1975-01-01

A separation method to provide reasonable yields of high specificity isoenzymes for the purpose of large scale, early clinical diagnosis of diseases and organic damage such as, myocardial infarction, hepatoma, muscular dystrophy, and infectous disorders is presented. Preliminary development plans are summarized. An analysis of required research and development and production resources is included. The costs of such resources and the potential profitability of a commercial space processing opportunity for electrophoretic separation of high specificity isoenzymes are reviewed.

Development of pseudo-linear gradient elution for high-throughput resin selectivity screening in RoboColumn® Format.

PubMed

Kiesewetter, André; Menstell, Peter; Peeck, Lars H; Stein, Andreas

2016-11-01

Rapid development of chromatographic processes relies on effective high-throughput screening (HTS) methods. This article describes the development of pseudo-linear gradient elution for resin selectivity screening using RoboColumns ® . It gives guidelines for the implementation of this HTS method on a Tecan Freedom EVO ® robotic platform, addressing fundamental aspects of scale down and liquid handling. The creation of a flexible script for buffer preparation and column operation plus efficient data processing provided the basis for this work. Based on the concept of discretization, linear gradient elution was transformed into multistep gradients. The impact of column size, flow rate, multistep gradient design, and fractionation scheme on separation efficiency was systematically investigated, using a ternary model protein mixture. We identified key parameters and defined optimal settings for effective column performance. For proof of concept, we examined the selectivity of several cation exchange resins using various buffer conditions. The final protocol enabled a clear differentiation of resin selectivity on miniature chromatography column (MCC) scale. Distinct differences in separation behavior of individual resins and the influence of buffer conditions could be demonstrated. Results obtained with the robotic platform were representative and consistent with data generated on a conventional chromatography system. A study on antibody monomer/high molecular weight separation comparing MCC and lab scale under higher loading conditions provided evidence of the applicability of the miniaturized approach to practically relevant feedstocks with challenging separation tasks as well as of the predictive quality for larger scale. A comparison of varying degrees of robotic method complexity with corresponding effort (analysis time and labware consumption) and output quality highlights tradeoffs to select a method appropriate for a given separation challenge or analytical constraints. © 2016 American Institute of Chemical Engineers Biotechnol. Prog., 32:1503-1519, 2016. © 2016 American Institute of Chemical Engineers.

Mars Atmospheric Capture and Gas Separation

NASA Technical Reports Server (NTRS)

Muscatello, Anthony; Santiago-Maldonado, Edgardo; Gibson, Tracy; Devor, Robert; Captain, James

2011-01-01

The Mars atmospheric capture and gas separation project is selecting, developing, and demonstrating techniques to capture and purify Martian atmospheric gases for their utilization for the production of hydrocarbons, oxygen, and water in ISRU systems. Trace gases will be required to be separated from Martian atmospheric gases to provide pure C02 to processing elements. In addition, other Martian gases, such as nitrogen and argon, occur in concentrations high enough to be useful as buffer gas and should be captured as welL To achieve these goals, highly efficient gas separation processes will be required. These gas separation techniques are also required across various areas within the ISRU project to support various consumable production processes. The development of innovative gas separation techniques will evaluate the current state-of-the-art for the gas separation required, with the objective to demonstrate and develop light-weight, low-power methods for gas separation. Gas separation requirements include, but are not limited to the selective separation of: (1) methane and water from un-reacted carbon oxides (C02- CO) and hydrogen typical of a Sabatier-type process, (2) carbon oxides and water from unreacted hydrogen from a Reverse Water-Gas Shift process, (3) carbon oxides from oxygen from a trash/waste processing reaction, and (4) helium from hydrogen or oxygen from a propellant scavenging process. Potential technologies for the separations include freezers, selective membranes, selective solvents, polymeric sorbents, zeolites, and new technologies. This paper and presentation will summarize the results of an extensive literature review and laboratory evaluations of candidate technologies for the capture and separation of C02 and other relevant gases.

A rapid method for soil cement design : Louisiana slope value method : part II : evaluation.

DOT National Transportation Integrated Search

1966-05-01

This report is an evaluation of the recently developed "Louisiana Slope Value Method". : The conclusion drawn are based on data from 637 separate samples representing nearly all major soil groups in Louisiana that are suitable for cement stabilizatio...

Separation and characterization of lignin from bio-ethanol production residue.

PubMed

Guo, Guowan; Li, Shujun; Wang, Lu; Ren, Shixue; Fang, Guizhen

2013-05-01

In order to develop an adequate method to separate lignin from bio-ethanol production residue, solvent extraction was conducted by using benzyl alcohol, dioxane and ethanol. Compared to the conventional alkali-solution and acid-isolation method, benzyl alcohol and dioxane extraction could reach higher lignin yield of 71.55% and 74.14% respectively. FTIR and XRD analysis results indicate that sodium hydroxide solution dissolved most of the lignin in the raw material. However, the low lignin yield by this method may be attributed to the products loss during the complex separation process. GPC and (1)H NMR results revealed that the dioxane-lignin had closer molecular weight with alkali-lignin, lower S/G ratio (0.22) and higher OHPh/OHAl ratio (0.45) with respect to benzyl alcohol-lignin. The results divulge that the lignin products separated from bio-ethanol production residue by dioxane extraction had fairly potential application with better chemical activity. Copyright © 2012 Elsevier Ltd. All rights reserved.

Lidar as a Diagnostic of Smoke/Obscurants: Overview and Assessment of the Development with Recommendations

DTIC Science & Technology

1984-10-03

aerosol , and the name " laser radar" is used to denote systems de- signed for the detection of solid objects...34* MEASUREMENW OF T(Li) BY SEPARATE TRANSMISSOMETER . One method of measuring * T(Li) is by a separate transmissometer system operating at the lidar wavelength... transmissometer path may be radially outward from the lidar (along the lidar beam) to save the expense of scanning hardware in a developing lidar system ,

Acoustic Microfluidics for Bioanalytical Application

NASA Astrophysics Data System (ADS)

Lopez, Gabriel

2013-03-01

This talk will present new methods the use of ultrasonic standing waves in microfluidic systems to manipulate microparticles for the purpose of bioassays and bioseparations. We have recently developed multi-node acoustic focusing flow cells that can position particles into many parallel flow streams and have demonstrated the potential of such flow cells in the development of high throughput, parallel flow cytometers. These experiments show the potential for the creation of high throughput flow cytometers in applications requiring high flow rates and rapid detection of rare cells. This talk will also present the development of elastomeric capture microparticles and their use in acoustophoretic separations. We have developed simple methods to form elastomeric particles that are surface functionalized with biomolecular recognition reagents. These compressible particles exhibit negative acoustic contrast in ultrasound when suspended in aqueous media, blood serum or diluted blood. These particles can be continuously separated from cells by flowing them through a microfluidic device that uses an ultrasonic standing wave to align the blood cells, which exhibit positive acoustic contrast, at a node in the acoustic pressure distribution while aligning the negative acoustic contrast elastomeric particles at the antinodes. Laminar flow of the separated particles to downstream collection ports allows for collection of the separated negative contrast particles and cells. Separated elastomeric particles were analyzed via flow cytometry to demonstrate nanomolar detection for prostate specific antigen in aqueous buffer and picomolar detection for IgG in plasma and diluted blood samples. This approach has potential applications in the development of rapid assays that detect the presence of low concentrations of biomarkers (including biomolecules and cells) in a number of biological sample types. We acknowledge support through the NSF Research Triangle MRSEC.

Chiral Separation of G-type Chemical Warfare Nerve Agents via Analytical Supercritical Fluid Chromatography

PubMed Central

Kasten, Shane A; Zulli, Steven; Jones, Jonathan L; Dephillipo, Thomas; Cerasoli, Douglas M

2014-01-01

Chemical warfare nerve agents (CWNAs) are extremely toxic organophosphorus compounds that contain a chiral phosphorus center. Undirected synthesis of G-type CWNAs produces stereoisomers of tabun, sarin, soman, and cyclosarin (GA, GB, GD, and GF, respectively). Analytical-scale methods were developed using a supercritical fluid chromatography (SFC) system in tandem with a mass spectrometer for the separation, quantitation, and isolation of individual stereoisomers of GA, GB, GD, and GF. Screening various chiral stationary phases (CSPs) for the capacity to provide full baseline separation of the CWNAs revealed that a Regis WhelkO1 (SS) column was capable of separating the enantiomers of GA, GB, and GF, with elution of the P(+) enantiomer preceding elution of the corresponding P(–) enantiomer; two WhelkO1 (SS) columns had to be connected in series to achieve complete baseline resolution. The four diastereomers of GD were also resolved using two tandem WhelkO1 (SS) columns, with complete baseline separation of the two P(+) epimers. A single WhelkO1 (RR) column with inverse stereochemistry resulted in baseline separation of the GD P(–) epimers. The analytical methods described can be scaled to allow isolation of individual stereoisomers to assist in screening and development of countermeasures to organophosphorus nerve agents. Chirality 26:817–824, 2014. © 2014 The Authors. Chirality published by John Wiley Periodicals, Inc. PMID:25298066

A method for the analysis of sugars in biological systems using reductive amination in combination with hydrophilic interaction chromatography and high resolution mass spectrometry.

PubMed

Bawazeer, Sami; Muhsen Ali, Ali; Alhawiti, Aliyah; Khalaf, Abedawn; Gibson, Colin; Tusiimire, Jonans; Watson, David G

2017-05-01

Separation of sugar isomers extracted from biological samples is challenging because of their natural occurrence as alpha and beta anomers and, in the case of hexoses, in their pyranose and furanose forms. A reductive amination method was developed for the tagging of sugars with the aim of it becoming part of a metabolomics work flow. The best separation of the common hexoses (glucose, fructose, mannose and galactose) was achieved when 2 H 5 -aniline was used as the tagging reagent in combination with separation on a ZICHILIC column. The method was used to tag a range of sugars including pentoses and uronic acids. The method was simple to perform and was able to improve both the separation of sugars and their response to electrospray ionisation. The method was applied to the profiling of sugars in urine where a number of hexose and pentose isomers could be observed. It was also applied to the quantification of sugars in post-mortem brain samples from three control samples and three samples from individuals who had suffered from bipolar disorder. Copyright © 2017 Elsevier B.V. All rights reserved.

Simultaneous determination of piracetam and its four impurities by RP-HPLC with UV detection.

PubMed

Arayne, M Saeed; Sultana, Najma; Siddiqui, Farhan Ahmed; Mirza, Agha Zeeshan; Qureshi, Faiza; Zuberi, M Hashim

2010-08-01

A simple and rapid high-performance liquid chromatographic method for the separation and determination of piracetam and its four impurities, 2-oxopyrrolidin-1-yl)acetic acid, pyrrolidin-2-one, methyl (2-oxopyrrolidin-1-yl)acetate, and ethyl (2-oxopyrrolidin-1-yl)acetate, was developed. The separation was achieved on a reversed-phase C(18) Nucleosil column (25 cm x 0.46 cm, 10 microm). The mobile phase is composed of an aqueous solution containing 0.2 g/L of triethyl amine-acetonitrile (85:15, v/v). The pH of the mobile phase was adjusted to 6.5 with phosphoric acid at a flow rate of 1 mL/min at ambient temperature and UV detection at 205 nm. The developed method was found to give good separation between the pure drug and its four related substance. The polynomial regression data for the calibration plots showed good linear relationship in the concentration range of 50-10,000 ng/mL, 25-10,000 ng/mL, 45-10,000 ng/mL, 34-10,000 ng/mL, and 55-10,000 ng/mL, respectively, with r(2) = 0.9999. The method was validated for precision, accuracy, ruggedness, and recovery. The minimum quantifiable amounts were found to be 50 ng/mL of piracetam, 25 ng/mL of 2-oxopyrrolidin-1-yl)acetic acid, 45 ng/mL of pyrrolidin-2-one, 34 ng/mL of methyl (2-oxopyrrolidin-1-yl)acetate, and 55 ng/mL of ethyl (2-oxopyrrolidin-1-yl)acetate. Statistical analysis proves that the method is reproducible and selective for the estimation of piracetam as well as its related substance. As the method could effectively separate the drug from the related substances, it can be employed as a stability-indicating one. The proposed method shows high efficiency, allowing the separation of the main component piracetam from other impurities.

Separated-pair independent particle model and the generalized Brillouin theorem: ab initio calculations on the dissociation of polyatomic molecules

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sundberg, Kenneth Randall

1976-01-01

A method is developed to optimize the separated-pair independent particle (SPIP) wave function; it is a special case of the separated-pair theory obtained by using two-term natural expansions of the geminals. The orbitals are optimized by a theory based on the generalized Brillouin theorem and iterative configuration interaction (CI) calculations in the space of the SPIP function and its single excitations. The geminal expansion coefficients are optimized by serial 2 x 2 CI calculations. Formulas are derived for the matrix elements. An algorithm to implement the method is presented, and the work needed to evaluate the molecular integrals is discussed.

Contributions of immunoaffinity chromatography to deep proteome profiling of human biofluids

DOE PAGES

Wu, Chaochao; Duan, Jicheng; Liu, Tao; ...

2016-01-12

Human biofluids, especially blood plasma or serum, hold great potential as the sources of candidate biomarkers for various diseases; however, the enormous dynamic range of protein concentrations in biofluids represents a significant analytical challenge for detecting promising low-abundance proteins. Over the last decade, various immunoaffinity chromatographic methods have been developed and routinely applied for separating low-abundance proteins from the high- and moderate-abundance proteins, thus enabling much more effective detection of low-abundance proteins. Herein, we review the advances of immunoaffinity separation methods and their contributions to the proteomic applications in human biofluids. The limitations and future perspectives of immunoaffinity separation methodsmore » are also discussed.« less

Recent developments in optical detection methods for microchip separations.

PubMed

Götz, Sebastian; Karst, Uwe

2007-01-01

This paper summarizes the features and performances of optical detection systems currently applied in order to monitor separations on microchip devices. Fluorescence detection, which delivers very high sensitivity and selectivity, is still the most widely applied method of detection. Instruments utilizing laser-induced fluorescence (LIF) and lamp-based fluorescence along with recent applications of light-emitting diodes (LED) as excitation sources are also covered in this paper. Since chemiluminescence detection can be achieved using extremely simple devices which no longer require light sources and optical components for focusing and collimation, interesting approaches based on this technique are presented, too. Although UV/vis absorbance is a detection method that is commonly used in standard desktop electrophoresis and liquid chromatography instruments, it has not yet reached the same level of popularity for microchip applications. Current applications of UV/vis absorbance detection to microchip separations and innovative approaches that increase sensitivity are described. This article, which contains 85 references, focuses on developments and applications published within the last three years, points out exciting new approaches, and provides future perspectives on this field.

State-of-the-art of recycling e-wastes by vacuum metallurgy separation.

PubMed

Zhan, Lu; Xu, Zhenming

2014-12-16

In recent era, more and more electric and electronic equipment wastes (e-wastes) are generated that contain both toxic and valuable materials in them. Most studies focus on the extraction of valuable metals like Au, Ag from e-wastes. However, the recycling of metals such as Pb, Cd, Zn, and organics has not attracted enough attentions. Vacuum metallurgy separation (VMS) processes can reduce pollution significantly using vacuum technique. It can effectively recycle heavy metals and organics from e-wastes in an environmentally friendly way, which is beneficial for both preventing the heavy metal contaminations and the sustainable development of resources. VMS can be classified into several methods, such as vacuum evaporation, vacuum carbon reduction and vacuum pyrolysis. This paper respectively reviews the state-of-art of these methods applied to recycling heavy metals and organics from several kinds of e-wastes. The method principle, equipment used, separating process, optimized operating parameters and recycling mechanism of each case are illustrated in details. The perspectives on the further development of e-wastes recycling by VMS are also presented.

MONTHLY REPORT OF DEVELOPMENT, SEPTEMBER 1963

DOE Office of Scientific and Technical Information (OSTI.GOV)

None

1964-10-31

Methods for separating germanium from Taiga carbonaceous shale by flotation and salt roasting are described. The recovery of vanadium from Beaverlodge mill tailings by carbonate leaching is briefly discussed. Methods of chemical analysis are also discussed. (N.W.R.)

Ketamine metabolites with antidepressant effects: Fast, economical, and eco-friendly enantioselective separation based on supercritical-fluid chromatography (SFC) and single quadrupole MS detection.

PubMed

Fassauer, Georg M; Hofstetter, Robert; Hasan, Mahmoud; Oswald, Stefan; Modeß, Christina; Siegmund, Werner; Link, Andreas

2017-11-30

Increasing evidence accumulates that metabolites of the dissociative anesthetic ketamine contribute considerably to the biological effects of this drug and could be developed as next generation antidepressants, especially for acute treatment of patients with therapy-refractory major depression. Analytical methods for the simultaneous determination of the plethora of hydroxylated, dehydrogenated and/or demethylated compounds formed after administration of ketamine hydrochloride are a prerequisite for future clinical investigations and a deeper understanding of the individual role of the isomers of these metabolites. In this study, we present development and validation of a method based on supercritical-fluid chromatography (SFC) coupled to single quadrupole MS detection that allows the separation of ketamine as well as all of its relevant metabolites detected in urine of healthy volunteers. Inherently to SFC methods, the run times of the novel protocol are four times shorter than in a comparable HPLC method, the use of organic solvents is reduced and we were able to demonstrate and validate the successful enantioselective separation and quantification of R- and S-ketamine, R- and S-norketamine, R- and S-dehydronorketamine and (2R,6R)- and (2S,6S)-hydroxynorketamine isomers differing in either constitution, stereochemistry, or both, in one run. The developed method may be useful in investigating the antidepressant efficacy of ketamine in clinical trials. Copyright © 2017 Elsevier B.V. All rights reserved.

QbD-oriented development and validation of a bioanalytical method for nevirapine with enhanced liquid-liquid extraction and chromatographic separation.

PubMed

Beg, Sarwar; Chaudhary, Vandna; Sharma, Gajanand; Garg, Babita; Panda, Sagar Suman; Singh, Bhupinder

2016-06-01

The present studies describe the systematic quality by design (QbD)-oriented development and validation of a simple, rapid, sensitive and cost-effective reversed-phase HPLC bioanalytical method for nevirapine in rat plasma. Chromatographic separation was carried out on a C18 column using isocratic 68:9:23% v/v elution of methanol, acetonitrile and water (pH 3, adjusted by orthophosphoric acid) at a flow rate of 1.0 mL/min using UV detection at 230 nm. A Box-Behnken design was applied for chromatographic method optimization taking mobile phase ratio, pH and flow rate as the critical method parameters (CMPs) from screening studies. Peak area, retention time, theoretical plates and peak tailing were measured as the critical analytical attributes (CAAs). Further, the bioanalytical liquid-liquid extraction process was optimized using an optimal design by selecting extraction time, centrifugation speed and temperature as the CMPs for percentage recovery of nevirapine as the CAA. The search for an optimum chromatographic solution was conducted through numerical desirability function. Validation studies performed as per the US Food and Drug Administration requirements revealed results within the acceptance limit. In a nutshell, the studies successfully demonstrate the utility of analytical QbD approach for the rational development of a bioanalytical method with enhanced chromatographic separation and recovery of nevirapine in rat plasma. Copyright © 2015 John Wiley & Sons, Ltd. Copyright © 2015 John Wiley & Sons, Ltd.

Accelerated in vitro release testing method for naltrexone loaded PLGA microspheres.

PubMed

Andhariya, Janki V; Choi, Stephanie; Wang, Yan; Zou, Yuan; Burgess, Diane J; Shen, Jie

2017-03-30

The objective of the present study was to develop a discriminatory and reproducible accelerated release testing method for naltrexone loaded parenteral polymeric microspheres. The commercially available naltrexone microsphere product (Vivitrol ® ) was used as the testing formulation in the in vitro release method development, and both sample-and-separate and USP apparatus 4 methods were investigated. Following an in vitro drug stability study, frequent media replacement and addition of anti-oxidant in the release medium were used to prevent degradation of naltrexone during release testing at "real-time" (37°C) and "accelerated" (45°C), respectively. The USP apparatus 4 method was more reproducible than the sample-and-separate method. In addition, the accelerated release profile obtained using USP apparatus 4 had a shortened release duration (within seven days), and good correlation with the "real-time" release profile. Lastly, the discriminatory ability of the developed accelerated release method was assessed using compositionally equivalent naltrexone microspheres with different release characteristics. The developed accelerated USP apparatus 4 release method was able to detect differences in the release characteristics of the prepared naltrexone microspheres. Moreover, a linear correlation was observed between the "real-time" and accelerated release profiles of all the formulations investigated, suggesting that the release mechanism(s) may be similar under both conditions. These results indicate that the developed accelerated USP apparatus 4 method has the potential to be an appropriate fast quality control tool for long-acting naltrexone PLGA microspheres. Copyright © 2017 Elsevier B.V. All rights reserved.

CE chips fabricated by injection molding and polyethylene/thermoplastic elastomer film packaging methods.

PubMed

Huang, Fu-Chun; Chen, Yih-Far; Lee, Gwo-Bin

2007-04-01

This study presents a new packaging method using a polyethylene/thermoplastic elastomer (PE/TPE) film to seal an injection-molded CE chip made of either poly(methyl methacrylate) (PMMA) or polycarbonate (PC) materials. The packaging is performed at atmospheric pressure and at room temperature, which is a fast, easy, and reliable bonding method to form a sealed CE chip for chemical analysis and biomedical applications. The fabrication of PMMA and PC microfluidic channels is accomplished by using an injection-molding process, which could be mass-produced for commercial applications. In addition to microfluidic CE channels, 3-D reservoirs for storing biosamples, and CE buffers are also formed during this injection-molding process. With this approach, a commercial CE chip can be of low cost and disposable. Finally, the functionality of the mass-produced CE chip is demonstrated through its successful separation of phiX174 DNA/HaeIII markers. Experimental data show that the S/N for the CE chips using the PE/TPE film has a value of 5.34, when utilizing DNA markers with a concentration of 2 ng/microL and a CE buffer of 2% hydroxypropyl-methylcellulose (HPMC) in Tris-borate-EDTA (TBE) with 1% YO-PRO-1 fluorescent dye. Thus, the detection limit of the developed chips is improved. Lastly, the developed CE chips are used for the separation and detection of PCR products. A mixture of an amplified antibiotic gene for Streptococcus pneumoniae and phiX174 DNA/HaeIII markers was successfully separated and detected by using the proposed CE chips. Experimental data show that these DNA samples were separated within 2 min. The study proposed a promising method for the development of mass-produced CE chips.

Determination of the antileukemic drug mitoguazone and seven other closely related bis(amidinohydrazones) in human blood serum by high-performance liquid chromatography.

PubMed

Koskinen, M; Elo, H; Lukkari, P; Riekkola, M L

1996-10-11

A reversed-phase (C18) HPLC method with diode-array detection was developed for the separation and determination of methylglyoxal bis(amidinohydrazone) (mitoguazone) and seven closely related aliphatic analogs thereof, namely the bis(amidinohydrazones) of glyoxal, dimethylglyoxal, ethylmethylglyoxal, methylpropylglyoxal, butylmethylglyoxal, diethylglyoxal and dipropylglyoxal. The mobile phase consisted of a non-linear binary gradient of methanol and 0.03 M aqueous sodium acetate buffer (pH 4.3). Good separation of the eight congeners was achieved. On increasing the methanol content of the eluent, the bis(amidinohydrazones) eluted in the order of increasing number of carbon atoms in the side-chains. The method was also applied to the quantitative analysis of the compounds in aqueous solution and, combined with ultrafiltration, for the separation of the eight congeners in spiked human blood serum. A separate simplified method for the quantitative determination of each of the compounds in spiked human blood serum samples was also developed. The methods developed made for the first time possible the simultaneous HPLC analysis of more than one bis(amidinohydrazones). The results obtained indicate that the bis(amidinohydrazones) studied obviously have a distinct tendency to form ion associates with acetate ions and probably also other carboxylate ions in aqueous solution. This aspect may be of biochemical significance, especially concerning the intracellular binding of the compounds. Each one of the compounds studied invariably gave rise to one peak only, this result supporting the theory that the conventional synthesis of each of the compounds gives rise to one geometrical isomer only. This result is completely in agreement with the results of previous proton and carbon NMR spectroscopic as well as X-ray diffraction studies.

Solid Phase Extraction (SPE) for Biodiesel Processing and Analysis

DTIC Science & Technology

2017-12-13

1 METHODS ...sources. There are several methods than can be applied to development of separation techniques that may replace necessary water wash steps in...biodiesel refinement. Unfortunately, the most common methods are poorly suited or face high costs when applied to diesel purification. Distillation is

Nanofiber/ZrO2-based mixed matrix separator for high safety/high-rate lithium-ion batteries

NASA Astrophysics Data System (ADS)

Xiao, Wei; Liu, Jianguo; Yan, Chuanwei

2017-10-01

A novel asymmetric separator based on a thin bacterial cellulose nanofiber (BCF)/nano-ZrO2 composite layer and a non-woven support was prepared by paper-making method. Owing to the relatively polar constituents and well-developed, gradient porous structure, the separator exhibited the advantages of higher thermal resistance, electrolyte wettability, and ionic conductivity in comparison to polyethylene separator. Based on these advantages, the Li/LiFePO4 cells assembled from this composite separator showed excellent performance characteristics, including outstanding C-rate capability, high capacity and cycling performance. Production of the composite separator is simple, environmentally benign and economically viable. Therefore, it's a good candidate for creating improved lithium-ion batteries.

Indirect ultraviolet detection of alkaline earth metal ions using an imidazolium ionic liquid as an ultraviolet absorption reagent in ion chromatography.

PubMed

Liu, Yong-Qiang; Yu, Hong

2017-04-01

A convenient and versatile method was developed for the separation and detection of alkaline earth metal ions by ion chromatography with indirect UV detection. The chromatographic separation of Mg 2+ , Ca 2+ , and Sr 2+ was performed on a carboxylic acid base cation exchange column using imidazolium ionic liquid/acid as the mobile phase, in which the imidazolium ionic liquid acted as an UV-absorption reagent. The effects of imidazolium ionic liquids, detection wavelength, acids in the mobile phase, and column temperature on the retention of Mg 2+ , Ca 2+ , and Sr 2+ were investigated. The main factors influencing the separation and detection were the background UV absorption reagent and the concentration of hydrogen ion in ion chromatography with indirect UV detection. The successful separation and detection of Mg 2+ , Ca 2+ , and Sr 2+ within 14 min were achieved using the selected chromatographic conditions, and the detection limits (S/N = 3) were 0.06, 0.12, and 0.23 mg/L, respectively. A new separation and detection method of alkaline earth metal ions by ion chromatography with indirect UV detection was developed, and the application range of ionic liquids was expanded. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Isotopic separation of acetaldehyde and methanol from their deuterated isotopologues on a porous layer open tubular column allows quantification by stable isotope dilution without mass spectrometric detection.

PubMed

Schmarr, Hans-Georg; Wacker, Michael; Mathes, Maximilian

2017-01-20

An isotopic separation of acetaldehyde and acetaldehyde-2,2,2-d3 was achieved in a temperature programmed run on a porous layer open tubular (PLOT) capillary column coated with particles of divinylbenzene ethylene glycol/dimethylacrylate (Rt ® -U-BOND). This is the prerequisite for the development of quantitative analytical methods based on a stable isotope dilution assay (SIDA) without a mass spectrometric detection (non-MS SIDA). For routine analysis a flame ionization detector (FID) can thus be applied as a robust and low-cost alternative. In a preliminary study, static headspace extraction and gas chromatographic separation (HS-GC-FID) of acetaldehyde in aqueous solutions was shown as an application. Good linearity was obtained in a calibration range from 0.4 to 40mgL -1 , with peak integration benefitting from the inverse isotope effect encountered on the specific porous polymer. Furthermore, separation of methanol and deuterated methanol (d3) could also be achieved under the same chromatographic conditions. The achieved isotopic separation of these important volatile compounds now allows non-MS SIDA-based methods that are still to be developed. Copyright © 2016 Elsevier B.V. All rights reserved.

Control of flow separation in a turbulent boundary layer

NASA Astrophysics Data System (ADS)

Cho, Minjeong; Choi, Sangho; Choi, Haecheon

2015-11-01

Towards the development of successful control methods for separation delay in a turbulent boundary layer, we adopt a model flow field, in which a turbulent separation occurs above a flat plate (Na and Moin 1998 JFM), and apply controls to this flow for reducing the size of the separation bubble and investigating the interaction between the forcing and flow near the separation bubble. We provide a single-frequency forcing with zero net mass flow rate at the upstream of the separation bubble. At low forcing frequencies, spanwise vortices are generated and travel downstream, bringing high momentum toward the wall and reducing the size of the separation bubble. Also, these vortices cause the separation and reattachment points to travel downstream. On the other hand, at high forcing frequencies, the size of the separation bubble becomes smaller and larger in time, respectively, due to the pressure gradient alternating favorably and adversely in time. Supported by NRF-2011-0028032 and 2014048162.

Detection of E. coli O157:H7 from ground beef using Fourier transform infrared (FT-IR) spectroscopy and chemometrics.

PubMed

Davis, Reeta; Irudayaraj, Joseph; Reuhs, Bradley L; Mauer, Lisa J

2010-08-01

FT-IR spectroscopy methods for detection, differentiation, and quantification of E. coli O157:H7 strains separated from ground beef were developed. Filtration and immunomagnetic separation (IMS) were used to extract live and dead E. coli O157:H7 cells from contaminated ground beef prior to spectral acquisition. Spectra were analyzed using chemometric techniques in OPUS, TQ Analyst, and WinDAS software programs. Standard plate counts were used for development and validation of spectral analyses. The detection limit based on a selectivity value using the OPUS ident test was 10(5) CFU/g for both Filtration-FT-IR and IMS-FT-IR methods. Experiments using ground beef inoculated with fewer cells (10(1) to 10(2) CFU/g) reached the detection limit at 6 h incubation. Partial least squares (PLS) models with cross validation were used to establish relationships between plate counts and FT-IR spectra. Better PLS predictions were obtained for quantifying live E. coli O157:H7 strains (R(2)> or = 0.9955, RMSEE < or = 0.17, RPD > or = 14) and different ratios of live and dead E. coli O157:H7 cells (R(2)= 0.9945, RMSEE = 2.75, RPD = 13.43) from ground beef using Filtration-FT-IR than IMS-FT-IR methods. Discriminant analysis and canonical variate analysis (CVA) of the spectra differentiated various strains of E. coli O157:H7 from an apathogenic control strain. CVA also separated spectra of 100% dead cells separated from ground beef from spectra of 0.5% live cells in the presence of 99.5% dead cells of E. coli O157:H7. These combined separation and FT-IR methods could be useful for rapid detection and differentiation of pathogens in complex foods.

Quantification of steviol glycosides in food products, Stevia leaves and formulations by planar chromatography, including proof of absence for steviol and isosteviol.

PubMed

Wald, Julian P; Morlock, Gertrud E

2017-07-14

Steviol glycosides may degrade in food products under certain processing and storage conditions. Hence, a method was developed that separated in the same chromatographic run seven important steviol glycosides, and additionally as a sum parameter, their reported breakdown products steviol and isosteviol. Through derivatizations with the 2-naphthol and the primuline reagent, the detection was selective and inexpensive. In case needed, the baseline separation of steviol and isosteviol was also demonstrated after a plate cut and subsequent short development (two-step method). The HPTLC method was robust with regard to varying sample matrix loads, as the stationary phase was used only once. A high sample throughput was achieved, i.e. 23 separations were performed in parallel on one plate. The total analysis time took 1h (30min application, 15min separation and 15min derivatization/densitometry) leading to a calculated analysis time of 2.6min per sample. The solvent consumption was 8mL in total (0.4mL per analysis). HPTLC-ESI-MS was employed for confirmation of the results obtained. Mass spectra were recorded only from the zones of interest, and not from matrix or background, leading to decisive advantages, such as less need for MS cleaning. The optimized HPTLC method was shown to effectively support quality control, as marketed samples may be falsified with cheaper synthetic sweeteners, which was also demonstrated in this study. The accuracy of the densitometric quantification in HPTLC was considered as high, as standards and samples were separated on fresh adsorbent and detected simultaneously under identical conditions, which minimized the influence of errors. Finally, the Aliivibrio fischeri bioassay was employed to obtain information on bioactive compounds in Stevia leaf extracts. Copyright © 2017 Elsevier B.V. All rights reserved.

Preparative separation and purification of steroidal saponins in Paris polyphylla var. yunnanensis by macroporous adsorption resins.

PubMed

Liu, Zhen; Wang, Jieyin; Gao, Wenyuan; Man, Shuli; Wang, Ying; Liu, Changxiao

2013-07-01

Saponins are active compounds in natural products. Many researchers have tried to find the method for knowing their concentration in herbs. Some methods, such as solid-liquid extraction and solvent extraction, have been developed. However, the extraction methods of the steroidal saponins from Paris polyphylla Smith var. yunnanensis (Liliaceae) are not fully researched. To establish a simple extraction method for the separation of steroidal saponins from the rhizomes of P. polyphylla Smith var. yunnanensis. Macroporous adsorption resins were used for the separation of steroidal saponins. To select the most suitable resins, seven kinds of macroporous resins were selected in this study. The static adsorption and desorption tests on macroporous resins were determined. Also, we optimized the temperature and the ethanol concentration in the extraction method by the contents of five kinds of saponins. Then, we compared the extraction method with two other methods. D101 resin demonstrated the best adsorption and desorption properties for steroidal saponins. Its adsorption data fits best to the Freundlich adsorption model. The contents of steroidal saponins in the product were 4.83-fold increased with recovery yields of 85.47%. The process achieved simple and effective enrichment and separation for steroidal saponins. The method provides a scientific basis for large-scale preparation of steroidal saponins from the Rhizoma Paridis and other plants.

Nonnegative matrix factorization: a blind sources separation method to extract content of fluorophores mixture media

NASA Astrophysics Data System (ADS)

Zhou, Kenneth J.; Chen, Jun

2014-03-01

The fluorophores of malignant human breast cells change their compositions that may be exposed in the fluorescence spectroscopy and blind source separation method. The content of the fluorophores mixture media such as tryptophan, collagen, elastin, NADH, and flavin were varied according to the cancer development. The native fluorescence spectra of these key fluorophores mixture media excited by the selective excitation wavelengths of 300 nm and 340 nm were analyzed using a blind source separation method: Nonnegative Matrix Factorization (NMF). The results show that the contribution from tryptophan, NADH and flavin to the fluorescence spectra of the mixture media is proportional to the content of each fluorophore. These data present a possibility that native fluorescence spectra decomposed by NMF can be used as potential native biomarkers for cancer detection evaluation of the cancer.

Separation of phospholipids in microfluidic chip device: application to high-throughput screening assays for lipid-modifying enzymes.

PubMed

Lin, Sansan; Fischl, Anthony S; Bi, Xiahui; Parce, Wally

2003-03-01

Phospholipid molecules such as ceramide and phosphoinositides play crucial roles in signal transduction pathways. Lipid-modifying enzymes including sphingomyelinase and phosphoinositide kinases regulate the generation and degradation of these lipid-signaling molecules and are important therapeutic targets in drug discovery. We now report a sensitive and convenient method to separate these lipids using microfluidic chip-based technology. The method takes advantage of the high-separation power of the microchips that separate lipids based on micellar electrokinetic capillary chromatography (MEKC) and the high sensitivity of fluorescence detection. We further exploited the method to develop a homogenous assay to monitor activities of lipid-modifying enzymes. The assay format consists of two steps: an on-plate enzymatic reaction using fluorescently labeled substrates followed by an on-chip MEKC separation of the reaction products from the substrates. The utility of the assay format for high-throughput screening (HTS) is demonstrated using phospholipase A(2) on the Caliper 250 HTS system: throughput of 80min per 384-well plate can be achieved with unattended running time of 5.4h. This enabling technology for assaying lipid-modifying enzymes is ideal for HTS because it avoids the use of radioactive substrates and complicated separation/washing steps and detects both substrate and product simultaneously.

Innovative high-performance liquid chromatography method development for the screening of 19 antimalarial drugs based on a generic approach, using design of experiments, independent component analysis and design space.

PubMed

Debrus, B; Lebrun, P; Kindenge, J Mbinze; Lecomte, F; Ceccato, A; Caliaro, G; Mbay, J Mavar Tayey; Boulanger, B; Marini, R D; Rozet, E; Hubert, Ph

2011-08-05

An innovative methodology based on design of experiments (DoE), independent component analysis (ICA) and design space (DS) was developed in previous works and was tested out with a mixture of 19 antimalarial drugs. This global LC method development methodology (i.e. DoE-ICA-DS) was used to optimize the separation of 19 antimalarial drugs to obtain a screening method. DoE-ICA-DS methodology is fully compliant with the current trend of quality by design. DoE was used to define the set of experiments to model the retention times at the beginning, the apex and the end of each peak. Furthermore, ICA was used to numerically separate coeluting peaks and estimate their unbiased retention times. Gradient time, temperature and pH were selected as the factors of a full factorial design. These retention times were modelled by stepwise multiple linear regressions. A recently introduced critical quality attribute, namely the separation criterion (S), was also used to assess the quality of separations rather than using the resolution. Furthermore, the resulting mathematical models were also studied from a chromatographic point of view to understand and investigate the chromatographic behaviour of each compound. Good adequacies were found between the mathematical models and the expected chromatographic behaviours predicted by chromatographic theory. Finally, focusing at quality risk management, the DS was computed as the multidimensional subspace where the probability for the separation criterion to lie in acceptance limits was higher than a defined quality level. The DS was computed propagating the prediction error from the modelled responses to the quality criterion using Monte Carlo simulations. DoE-ICA-DS allowed encountering optimal operating conditions to obtain a robust screening method for the 19 considered antimalarial drugs in the framework of the fight against counterfeit medicines. Moreover and only on the basis of the same data set, a dedicated method for the determination of three antimalarial compounds in a pharmaceutical formulation was optimized to demonstrate both the efficiency and flexibility of the methodology proposed in the present study. Copyright © 2011 Elsevier B.V. All rights reserved.

Robust water fat separated dual-echo MRI by phase-sensitive reconstruction.

PubMed

Romu, Thobias; Dahlström, Nils; Leinhard, Olof Dahlqvist; Borga, Magnus

2017-09-01

The purpose of this work was to develop and evaluate a robust water-fat separation method for T1-weighted symmetric two-point Dixon data. A method for water-fat separation by phase unwrapping of the opposite-phase images by phase-sensitive reconstruction (PSR) is introduced. PSR consists of three steps; (1), identification of clusters of tissue voxels; (2), unwrapping of the phase in each cluster by solving Poisson's equation; and (3), finding the correct sign of each unwrapped opposite-phase cluster, so that the water-fat images are assigned the correct identities. Robustness was evaluated by counting the number of water-fat swap artifacts in a total of 733 image volumes. The method was also compared to commercial software. In the water-fat separated image volumes, the PSR method failed to unwrap the phase of one cluster and misclassified 10. One swap was observed in areas affected by motion and was constricted to the affected area. Twenty swaps were observed surrounding susceptibility artifacts, none of which spread outside the artifact affected regions. The PSR method had fewer swaps when compared to commercial software. The PSR method can robustly produce water-fat separated whole-body images based on symmetric two-echo spoiled gradient echo images, under both ideal conditions and in the presence of common artifacts. Magn Reson Med 78:1208-1216, 2017. © 2016 International Society for Magnetic Resonance in Medicine. © 2016 International Society for Magnetic Resonance in Medicine.

Mesenchymal-epithelial interaction techniques

PubMed Central

Baskin, Lawrence

2016-01-01

This paper reviews the importance of mesenchymal-epithelial interactions in development and gives detailed technical protocols for investigating these interactions. Successful analysis of mesenchymal-epithelial interactions requires knowing the ages in which embryonic, neonatal and adult organs can be separated into mesenchymal and epithelial tissues. Methods for separation of mesenchymal and epithelial and preparation of tissue recombinants are described. PMID:26610327

Quality evaluation of Guan-Xin-Ning injection based on fingerprint analysis and simultaneous separation and determination of seven bioactive constituents by capillary electrophoresis.

PubMed

Xu, Liying; Chang, Ruimiao; Chen, Meng; Li, Lou; Huang, Yayun; Zhang, Hongfen; Chen, Anjia

2017-12-01

The purpose of this study was to develop a comprehensive, rapid and practical capillary electrophoresis (CE) method for quality control (QC) of Guan-Xin-Ning (GXN) injection based on fingerprint analysis and simultaneous separation and determination of seven constituents. In fingerprint analysis, a capillary zone electrophoresis (CZE) method with a running buffer of 30 mM borate solution (pH 9.3) was established. Meanwhile, ten batches of samples were used to establish the fingerprint electropherogram and 34 common peaks were obtained within 20 min. The RSD of relative migration times (RMT) and relative peak areas (RPA) were less than 5%. In order to further evaluate the quality of GXN injection, a micellar electrokinetic chromatography (MEKC) method was developed for simultaneous separation and determination of bioactive constituents. Seven components reached baseline separation with a running buffer containing 35 mM SDS and 45 mM borate solution (pH 9.3). A good linearity was obtained with correlation coefficients from 0.9906 to 0.9997. The LOD and LOQ ranged from 0.12 to 1.50 μg/mL and from 0.40 to 4.90 μg/mL, respectively. The recoveries ranged between 99.0 and 104.4%. Therefore, it was concluded that the proposed method can be used for full-scale quality analysis of GXN injection. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Method Development in Forensic Toxicology.

PubMed

Peters, Frank T; Wissenbach, Dirk K; Busardo, Francesco Paolo; Marchei, Emilia; Pichini, Simona

2017-01-01

In the field of forensic toxicology, the quality of analytical methods is of great importance to ensure the reliability of results and to avoid unjustified legal consequences. A key to high quality analytical methods is a thorough method development. The presented article will provide an overview on the process of developing methods for forensic applications. This includes the definition of the method's purpose (e.g. qualitative vs quantitative) and the analytes to be included, choosing an appropriate sample matrix, setting up separation and detection systems as well as establishing a versatile sample preparation. Method development is concluded by an optimization process after which the new method is subject to method validation. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

The challenges of simulating wake vortex encounters and assessing separation criteria

NASA Technical Reports Server (NTRS)

Dunham, R. E.; Stuever, Robert A.; Vicroy, Dan D.

1993-01-01

During landings and take-offs, the longitudinal spacing between airplanes is in part determined by the safe separation required to avoid the trailing vortex wake of the preceding aircraft. Safe exploration of the feasibility of reducing longitudinal separation standards will require use of aircraft simulators. This paper discusses the approaches to vortex modeling, methods for modeling the aircraft/vortex interaction, some of the previous attempts of defining vortex hazard criteria, and current understanding of the development of vortex hazard criteria.

Simple, rapid, and environmentally friendly method for the separation of isoflavones using ultra-high performance supercritical fluid chromatography.

PubMed

Wu, Wenjie; Zhang, Yuan; Wu, Hanqiu; Zhou, Weie; Cheng, Yan; Li, Hongna; Zhang, Chuanbin; Li, Lulu; Huang, Ying; Zhang, Feng

2017-07-01

Isoflavones are natural substances that exhibit hormone-like pharmacological activities. The separation of isoflavones remains an analytical challenge because of their similar structures. We show that ultra-high performance supercritical fluid chromatography can be an appropriate tool to achieve the fast separation of 12 common dietary isoflavones. Among the five tested columns the Torus DEA column was found to be the most effective column for the separation of these isoflavones. The impact of individual parameters on the retention time and separation factor was evaluated. These parameters were optimized to develop a simple, rapid, and green method for the separation of the 12 target analytes. It only took 12.91 min using gradient elution with methanol as an organic modifier and formic acid as an additive. These isoflavones were determined with limit of quantitation ranging from 0.10 to 0.50 μg/mL, which was sufficient for reliable determination of various matrixes. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Proceedings of the First Hanford Separation Science Workshop

DOE Office of Scientific and Technical Information (OSTI.GOV)

Not Available

1993-05-01

The First Hanford Separation Science Workshop, sponsored by PNL had two main objectives: (1) assess the applicability of available separation methods for environmental restoration and for minimization, recovery, and recycle of mixed and radioactive mutes; and (2) identify research needs that must be addressed to create new or improved technologies. The information gathered at this workshop not only applies to Hanford but could be adapted to DOE facilities throughout the nation as well. These proceedings have been divided into three components: Background and Introduction to the Problem gives an overview of the history of the Site and the cleanup mission,more » including waste management operations, past disposal practices, current operations, and plans for the future. Also included in this section is a discussion of specific problems concerning the chemistry of the Hanford wastes. Separation Methodologies contains the papers given at the workshop by national experts in the field of separation science regarding the state-of-the-art of various methods and their applicability/adaptability to Hanford. Research Needs identifies further research areas developed in working group sessions. Individual papers are indexed separately.« less

High-resolution Identification and Separation of Living Cell Types by Multiple microRNA-responsive Synthetic mRNAs.

PubMed

Endo, Kei; Hayashi, Karin; Saito, Hirohide

2016-02-23

The precise identification and separation of living cell types is critical to both study cell function and prepare cells for medical applications. However, intracellular information to distinguish live cells remains largely inaccessible. Here, we develop a method for high-resolution identification and separation of cell types by quantifying multiple microRNA (miRNA) activities in live cell populations. We found that a set of miRNA-responsive, in vitro synthesized mRNAs identify a specific cell population as a sharp peak and clearly separate different cell types based on less than two-fold differences in miRNA activities. Increasing the number of miRNA-responsive mRNAs enhanced the capability for cell identification and separation, as we precisely and simultaneously distinguished different cell types with similar miRNA profiles. In addition, the set of synthetic mRNAs separated HeLa cells into subgroups, uncovering heterogeneity of the cells and the level of resolution achievable. Our method could identify target live cells and improve the efficiency of cell purification from heterogeneous populations.

Industrial application of green chromatography--I. Separation and analysis of niacinamide in skincare creams using pure water as the mobile phase.

PubMed

Yang, Yu; Strickland, Zackary; Kapalavavi, Brahmam; Marple, Ronita; Gamsky, Chris

2011-03-15

In this work, chromatographic separation of niacin and niacinamide using pure water as the sole component in the mobile phase has been investigated. The separation and analysis of niacinamide have been optimized using three columns at different temperatures and various flow rates. Our results clearly demonstrate that separation and analysis of niacinamide from skincare products can be achieved using pure water as the eluent at 60°C on a Waters XTerra MS C18 column, a Waters XBridge C18 column, or at 80°C on a Hamilton PRP-1 column. The separation efficiency, quantification quality, and analysis time of this new method are at least comparable with those of the traditional HPLC methods. Compared with traditional HPLC, the major advantage of this newly developed green chromatography technique is the elimination of organic solvents required in the HPLC mobile phase. In addition, the pure water chromatography separations described in this work can be directly applied in industrial plant settings without further modification of the existing HPLC equipment. Copyright © 2011 Elsevier B.V. All rights reserved.

Isolation, Separation, and Preconcentration of Biologically Active Compounds from Plant Matrices by Extraction Techniques.

PubMed

Raks, Victoria; Al-Suod, Hossam; Buszewski, Bogusław

2018-01-01

Development of efficient methods for isolation and separation of biologically active compounds remains an important challenge for researchers. Designing systems such as organomineral composite materials that allow extraction of a wide range of biologically active compounds, acting as broad-utility solid-phase extraction agents, remains an important and necessary task. Selective sorbents can be easily used for highly selective and reliable extraction of specific components present in complex matrices. Herein, state-of-the-art approaches for selective isolation, preconcentration, and separation of biologically active compounds from a range of matrices are discussed. Primary focus is given to novel extraction methods for some biologically active compounds including cyclic polyols, flavonoids, and oligosaccharides from plants. In addition, application of silica-, carbon-, and polymer-based solid-phase extraction adsorbents and membrane extraction for selective separation of these compounds is discussed. Potential separation process interactions are recommended; their understanding is of utmost importance for the creation of optimal conditions to extract biologically active compounds including those with estrogenic properties.

Centrifugal partition chromatography enables selective enrichment of trimeric and tetrameric proanthocyanidins for biomaterial development.

PubMed

Phansalkar, Rasika S; Nam, Joo-Won; Chen, Shao-Nong; McAlpine, James B; Leme, Ariene A; Aydin, Berdan; Bedran-Russo, Ana-Karina; Pauli, Guido F

2018-02-02

Proanthocyanidins (PACs) find wide applications for human use including food, cosmetics, dietary supplements, and pharmaceuticals. The chemical complexity associated with PACs has triggered the development of various chromatographic techniques, with countercurrent separation (CCS) gaining in popularity. This study applied the recently developed DESIGNER (Depletion and Enrichment of Select Ingredients Generating Normalized Extract Resources) approach for the selective enrichment of trimeric and tetrameric PACs using centrifugal partition chromatography (CPC). This CPC method aims at developing PAC based biomaterials, particularly for their application in restoring and repairing dental hard tissue. A general separation scheme beginning with the depletion of polymeric PACs, followed by the removal of monomeric flavan-3-ols and a final enrichment step produced PAC trimer and tetramer enriched fractions. A successful application of this separation scheme is demonstrated for four polyphenol rich plant sources: grape seeds, pine bark, cinnamon bark, and cocoa seeds. Minor modifications to the generic DESIGNER CCS method were sufficient to accommodate the varying chemical complexities of the individual source materials. The step-wise enrichment of PAC trimers and tetramers was monitored using normal phase TLC and Diol-HPLC-UV analyses. CPC proved to be a reliable tool for the selective enrichment of medium size oligomeric PACs (OPACs). This method plays a key role in the development of dental biomaterials considering its reliability and reproducibility, as well as its scale-up capabilities for possible larger-scale manufacturing. Copyright © 2017 Elsevier B.V. All rights reserved.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Schneider, T

Purpose: Since 2008 the Physikalisch-Technische Bundesanstalt (PTB) has been offering the calibration of {sup 125}I-brachytherapy sources in terms of the reference air-kerma rate (RAKR). The primary standard is a large air-filled parallel-plate extrapolation chamber. The measurement principle is based on the fact that the air-kerma rate is proportional to the increment of ionization per increment of chamber volume at chamber depths greater than the range of secondary electrons originating from the electrode x{sub 0}. Methods: Two methods for deriving the RAKR from the measured ionization charges are: (1) to determine the RAKR from the slope of the linear fit tomore » the so-called ’extrapolation curve’, the measured ionization charges Q vs. plate separations x or (2) to differentiate Q(x) and to derive the RAKR by a linear extrapolation towards zero plate separation. For both methods, correcting the measured data for all known influencing effects before the evaluation method is applied is a precondition. However, the discrepancy of their results is larger than the uncertainty given for the determination of the RAKR with both methods. Results: A new approach to derive the RAKR from the measurements is investigated as an alternative. The method was developed from the ground up, based on radiation transport theory. A conversion factor C(x{sub 1}, x{sub 2}) is applied to the difference of charges measured at the two plate separations x{sub 1} and x{sub 2}. This factor is composed of quotients of three air-kerma values calculated for different plate separations in the chamber: the air kerma Ka(0) for plate separation zero, and the mean air kermas at the plate separations x{sub 1} and x{sub 2}, respectively. The RAKR determined with method (1) yields 4.877 µGy/h, and with method (2) 4.596 µGy/h. The application of the alternative approach results in 4.810 µGy/h. Conclusion: The alternative method shall be established in the future.« less

A rapid method for the sequential separation of polonium, plutonium, americium and uranium in drinking water.

PubMed

Lemons, B; Khaing, H; Ward, A; Thakur, P

2018-06-01

A new sequential separation method for the determination of polonium and actinides (Pu, Am and U) in drinking water samples has been developed that can be used for emergency response or routine water analyses. For the first time, the application of TEVA chromatography column in the sequential separation of polonium and plutonium has been studied. This method utilizes a rapid Fe +3 co-precipitation step to remove matrix interferences, followed by plutonium oxidation state adjustment to Pu 4+ and an incubation period of ~ 1 h at 50-60 °C to allow Po 2+ to oxidize to Po 4+ . The polonium and plutonium were then separated on a TEVA column, while separation of americium from uranium was performed on a TRU column. After separation, polonium was micro-precipitated with copper sulfide (CuS), while actinides were micro co-precipitated using neodymium fluoride (NdF 3 ) for counting by the alpha spectrometry. The method is simple, robust and can be performed quickly with excellent removal of interferences, high chemical recovery and very good alpha peak resolution. The efficiency and reliability of the procedures were tested by using spiked samples. The effect of several transition metals (Cu 2+ , Pb 2+ , Fe 3+ , Fe 2+ , and Ni 2+ ) on the performance of this method were also assessed to evaluate the potential matrix effects. Studies indicate that presence of up to 25 mg of these cations in the samples had no adverse effect on the recovery or the resolution of polonium alpha peaks. Copyright © 2018 Elsevier Ltd. All rights reserved.

Different Spectrophotometric and Chromatographic Methods for Determination of Mepivacaine and Its Toxic Impurity.

PubMed

Abdelwahab, Nada S; Fared, Nehal F; Elagawany, Mohamed; Abdelmomen, Esraa H

2017-09-01

Stability-indicating spectrophotometric, TLC-densitometric, and ultra-performance LC (UPLC) methods were developed for the determination of mepivacaine HCl (MEP) in the presence of its toxic impurity, 2,6-dimethylanaline (DMA). Different spectrophotometric methods were developed for the determination of MEP and DMA. In a dual-wavelength method combined with direct spectrophotometric measurement, the absorbance difference between 221.4 and 240 nm was used for MEP measurements, whereas the absorbance at 283 nm was used for measuring DMA in the binary mixture. In the second-derivative method, amplitudes at 272.2 and 232.6 nm were recorded and used for the determination of MEP and DMA, respectively. The developed TLC-densitometric method depended on chromatographic separation using silica gel 60 F254 TLC plates as a stationary phase and methanol-water-acetic acid (9 + 1 + 0.1, v/v/v) as a developing system, with UV scanning at 230 nm. The developed UPLC method depended on separation using a C18 column (250 × 4.6 mm id, 5 μm particle size) as a stationary phase and acetonitrile-water (40 + 60, v/v; pH 4 with phosphoric acid) as a mobile phase at a flow rate of 0.4 mL/min, with UV detection at 215 nm. The chromatographic run time was approximately 1 min. The proposed methods were validated with respect to International Conference on Harmonization guidelines regarding precision, accuracy, ruggedness, robustness, and specificity.

Stability-Indicating TLC-Densitometric and HPLC Methods for the Simultaneous Determination of Piracetam and Vincamine in the Presence of Their Degradation Products.

PubMed

Ahmed, Amal B; Abdelrahman, Maha M; Abdelwahab, Nada S; Salama, Fathy M

2016-11-01

Newly established TLC-densitometric and RP-HPLC methods were developed and validated for the simultaneous determination of Piracetam (PIR) and Vincamine (VINC) in their pharmaceutical formulation and in the presence of PIR and VINC degradation products, PD and VD, respectively. The proposed TLC-densitometric method is based on the separation and quantitation of the studied components using a developing system that consists of chloroform-methanol-glacial acetic acid-triethylamine (8 + 2 + 0.1 + 0.1, v/v/v/v) on TLC silica gel 60 F254 plates, followed by densitometric scanning at 230 nm. On the other hand, the developed RP-HPLC method is based on the separation of the studied components using an isocratic elution of 0.05 M KH2PO4 (containing 0.1% triethylamine adjusted to pH 3 with orthophosphoric acid)-methanol (95 + 5, v/v) on a C8 column at a flow rate of 1 mL/min with diode-array detection at 230 nm. The developed methods were validated according to International Conference on Harmonization guidelines and demonstrated good accuracy and precision. Moreover, the developed TLC-densitometric and RP-HPLC methods are suitable as stability-indicating assay methods for the simultaneous determination of PD and VD either in bulk powder or pharmaceutical formulation. The results were statistically compared with those obtained by the reported RP-HPLC method using t- and F-tests.

Rapid methods for the isolation of actinides Sr, Tc and Po from raw urine.

PubMed

McAlister, Daniel R; Horwitz, E Philip; Harvey, James T

2011-08-01

Rapid methods for the isolation and analysis of individual actinides (Th, U, Pu, Am/Cm) and Sr, Tc and Po from small volumes of raw urine have been developed. The methods involve acidification of the sample and the addition of aluminum nitrate or aluminum chloride salting-out agent prior to isolation of the desired analyte using a tandem combination of prefilter material and extraction chromatographic resin. The method has been applied to the separation of individual analytes from spiked urine samples. Analytes were recovered in high yield and radionuclide purity with separation times as low as 30 min. The chemistry employed is compatible with automation on the ARSIIe instrument.

Hybrid microfluidics combined with active and passive approaches for continuous cell separation.

PubMed

Yan, Sheng; Zhang, Jun; Yuan, Dan; Li, Weihua

2017-01-01

Microfluidics, which is classified as either active or passive, is capable of separating cells of interest from a complex and heterogeneous sample. Active methods utilise external fields such as electric, magnetic, acoustic, and optical to drive cells for separation, while passive methods utilise channel structures, intrinsic hydrodynamic forces, and steric hindrances to manipulate cells. However, when processing complex biological samples such as whole blood with rare cells, separation with a single module microfluidic device is difficult. Hybrid microfluidics is an emerging technique, which utilises active and passive methods whilst fulfilling higher requirements for stable performance, versatility, and convenience, including (i) the ability to process multi-target cells, (ii) enhanced ability for multiplexed separation, (iii) higher sensitivity, and (iv) tunability for a wider operational range. This review introduces the fundamental physics and typical formats for subclasses of hybrid microfluidic devices based on their different physical fields; presents current examples of cell sorting to highlight the advantage and usefulness of hybrid microfluidics on biomedicine, and then discusses the challenges and perspective of future development and the promising direction of research in this field. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Inverse transonic airfoil design methods including boundary layer and viscous interaction effects

NASA Technical Reports Server (NTRS)

Carlson, L. A.

1979-01-01

The development and incorporation into TRANDES of a fully conservative analysis method utilizing the artificial compressibility approach is described. The method allows for lifting cases and finite thickness airfoils and utilizes a stretched coordinate system. Wave drag and massive separation studies are also discussed.

Aeroelastic loads prediction for an arrow wing. Task 1: Evaluation of R. P. White's method

NASA Technical Reports Server (NTRS)

Borland, C. J.; Manro, M. E.

1983-01-01

The separated flow method is evaluated. This method was developed for moderately swept wings with multiple, constant strength vortex systems. The flow on the highly swept wing used in this evaluation is characterized by a single vortex system of continuously varying strength.

Recent theoretical developments and experimental studies pertinent to vortex flow aerodynamics - With a view towards design

NASA Technical Reports Server (NTRS)

Lamar, J. E.; Luckring, J. M.

1978-01-01

A review is presented of recent progress in a research program directed towards the development of an improved vortex-flow technology base. It is pointed out that separation induced vortex-flows from the leading and side edges play an important role in the high angle-of-attack aerodynamic characteristics of a wide range of modern aircraft. In the analysis and design of high-speed aircraft, a detailed knowledge of this type of separation is required, particularly with regard to critical wind loads and the stability and performance at various off-design conditions. A description of analytical methods is presented. The theoretical methods employed are divided into two classes which are dependent upon the underlying aerodynamic assumptions. One conical flow method is considered along with three different nonconical flow methods. Comparisons are conducted between the described methods and available aerodynamic data. Attention is also given to a vortex flow drag study and a vortex flow wing design using suction analogy.

The development of methods for the detection of Salmonella in chickens by a combination of immunomagnetic separation and PCRs.

PubMed

Dai, Fengying; Zhang, Miao; Xu, Dixin; Yang, Yin; Wang, Jiaxiao; Li, Mingzhen; Du, Meihong

2017-11-01

Micro- and nanoimmunomagnetic beads (MIMBs and NIMBs) used for immunomagnetic separation (IMS) with PCR were studied for the rapid detection of Salmonella. The capture efficiency of the two different IMBs was evaluated by a conventional plate counting method, and the binding pattern was studied using scanning electron microscopy. The specificity of the IMBs was tested with Salmonella, Shigella flexneri, enterohemorrhagic Escherichia coli O157:H7, and Listeria monocytogenes. By comparing the pre-enrichment IMS and the IMS enrichment steps with a 5.5-H enrichment time, this study developed a rapid and sensitive method for the detection of Salmonella in chicken. The method was implemented by IMS enrichment and PCR with MIMBs and NIMBs, with a total analysis time of 8 H. We showed that the method was sensitive based on NIMBs with a detection limit of 10° CFU for Salmonella in 25 g of chicken. © 2016 International Union of Biochemistry and Molecular Biology, Inc.

Neutral monosaccharide composition analysis of plant-derived oligo- and polysaccharides by high performance liquid chromatography.

PubMed

Yan, Jun; Shi, Songshan; Wang, Hongwei; Liu, Ruimin; Li, Ning; Chen, Yonglin; Wang, Shunchun

2016-01-20

A novel analytical method for neutral monosaccharide composition analysis of plant-derived oligo- and polysaccharides was developed using hydrophilic interaction liquid chromatography coupled to a charged aerosol detector. The effects of column type, additives, pH and column temperature on retention and separation were evaluated. Additionally, the method could distinguish potential impurities in samples, including chloride, sulfate and sodium, from sugars. The results of validation demonstrated that this method had good linearity (R(2) ≥ 0.9981), high precision (relative standard deviation ≤ 4.43%), and adequate accuracy (94.02-103.37% recovery) and sensitivity (detection limit: 15-40 ng). Finally, the monosaccharide compositions of the polysaccharide from Eclipta prostrasta L. and stachyose were successfully profiled through this method. This report represents the first time that all of these common monosaccharides could be well-separated and determined simultaneously by high performance liquid chromatography without additional derivatization. This newly developed method is convenient, efficient and reliable for monosaccharide analysis. Copyright © 2015 Elsevier Ltd. All rights reserved.

Accomplishing simple, solubility-based separations of rare earth elements with complexes bearing size-sensitive molecular apertures

PubMed Central

Bogart, Justin A.; Cole, Bren E.; Boreen, Michael A.; Lippincott, Connor A.; Manor, Brian C.; Carroll, Patrick J.; Schelter, Eric J.

2016-01-01

Rare earth (RE) metals are critical components of electronic materials and permanent magnets. Recycling of consumer materials is a promising new source of rare REs. To incentivize recycling, there is a clear need for the development of simple methods for targeted separations of mixtures of RE metal salts. Metal complexes of a tripodal hydroxylaminato ligand, TriNOx3–, featured a size-sensitive aperture formed of its three η2-(N,O) ligand arms. Exposure of cations in the aperture induced a self-associative equilibrium comprising RE(TriNOx)THF and [RE(TriNOx)]2 species. Differences in the equilibrium constants Kdimer for early and late metals enabled simple separations through leaching. Separations were performed on RE1/RE2 mixtures, where RE1 = La–Sm and RE2 = Gd–Lu, with emphasis on Eu/Y separations for potential applications in the recycling of phosphor waste from compact fluorescent light bulbs. Using the leaching method, separations factors approaching 2,000 were obtained for early–late RE combinations. Following solvent optimization, >95% pure samples of Eu were obtained with a 67% recovery for the technologically relevant Eu/Y separation. PMID:27956636

Accomplishing simple, solubility-based separations of rare earth elements with complexes bearing size-sensitive molecular apertures.

PubMed

Bogart, Justin A; Cole, Bren E; Boreen, Michael A; Lippincott, Connor A; Manor, Brian C; Carroll, Patrick J; Schelter, Eric J

2016-12-27

Rare earth (RE) metals are critical components of electronic materials and permanent magnets. Recycling of consumer materials is a promising new source of rare REs. To incentivize recycling, there is a clear need for the development of simple methods for targeted separations of mixtures of RE metal salts. Metal complexes of a tripodal hydroxylaminato ligand, TriNOx 3- , featured a size-sensitive aperture formed of its three η 2 -(N,O) ligand arms. Exposure of cations in the aperture induced a self-associative equilibrium comprising RE(TriNOx)THF and [RE(TriNOx)] 2 species. Differences in the equilibrium constants K dimer for early and late metals enabled simple separations through leaching. Separations were performed on RE1/RE2 mixtures, where RE1 = La-Sm and RE2 = Gd-Lu, with emphasis on Eu/Y separations for potential applications in the recycling of phosphor waste from compact fluorescent light bulbs. Using the leaching method, separations factors approaching 2,000 were obtained for early-late RE combinations. Following solvent optimization, >95% pure samples of Eu were obtained with a 67% recovery for the technologically relevant Eu/Y separation.

Thermally assisted acoustophoresis as a new stiffness-based separation method

NASA Astrophysics Data System (ADS)

Dolatmoradi, Ata; El-Zahab, Bilal

2017-02-01

The use of acoustophoretic separation devices provides a feasible means in biomedical diagnostics for label-free separation of diseased cells. Separation via acoustophoresis, however, has been restricted mainly to size contrast. Thermally-assisted acoustophoresis, as a newly-developed approach, integrates acoustic and thermal actuators on the same platform, enabling a stiffness-based separation when adjusted properly. Using this method, we have demonstrated the possibility of separating cell-mimicking liposomes based on their membrane stiffness. In a temperature-tuned microchannel with an overlaid ultrasonic standing wave, the acoustic contrast factor of a liposome is mainly determined according to its compressibility compared to that of medium. The sign of this factor was observed to flip to a negative value at a specific temperature, unique to the composition of the liposome. This sign switch was hypothesized to be due to the thermotropic phase transitions in the liposome's membrane upon which an apparent effect on the compressibility is experienced by the liposome. By choosing the midpoint of the existing temperature window for two different compositions, within which liposomes were mechanically distinct enough to become differentiable in the acoustic radiation field, we examined the separation efficiency under different flow rate conditions.

A review of oxygen removal from oxygen-bearing coal-mine methane.

PubMed

Zhao, Peiyu; Zhang, Guojie; Sun, Yinghui; Xu, Ying

2017-06-01

In this article, a comparison will be made concerning the advantages and disadvantages of five kinds of coal mine methane (CMM) deoxygenation method, including pressure swing adsorption, combustion, membrane separation, non-metallic reduction, and cryogenic distillation. Pressure swing adsorption has a wide range of application and strong production capacity. To achieve this goal, adsorbent must have high selectivity, adsorption capacity, and adequate adsorption/desorption kinetics, remain stable after several adsorption/desorption cycles, and possess good thermal and mechanical stabilities. Catalytic combustion deoxygenation is a high-temperature exothermic redox chemical reaction, which releases large amounts of thermal energy. So, the stable and accurate control of the temperature is not easy. Meanwhile partial methane is lost. The key of catalytic combustion deoxygenation lies in the development of high-efficiency catalyst. Membrane separation has advantages of high separation efficiency and low energy consumption. However, there are many obstacles, including higher costs. Membrane materials have the requirements of both high permeability and high selectivity. The development of new membrane materials is a key for membrane separation. Cryogenic distillation has many excellence advantages, such as high purity production and high recovery. However, the energy consumption increases with decreasing CH 4 concentrations in feed gas. Moreover, there are many types of operational security problems. And that several kinds of deoxygenation techniques mentioned above have an economic value just for oxygen-bearing CMM with methane content above 30%. Moreover, all the above methods are not applicable to deoxygenation of low concentration CMM. Non-metallic reduction method cannot only realize cyclic utilization of deoxidizer but also have no impurity gases generation. It also has a relatively low cost and low loss rate of methane, and the oxygen is removed thoroughly. In particular, the non-metallic reduction method has good development prospects for low concentration oxygen-bearing CMM. This article also points out the direction of future development of coal mine methane deoxygenation.

Preparative scale separation of thulium from erbium for neutron capture cross section measurements - Part: Preparative scale

DOE PAGES

Birnbaum, Eva R.; Bene, Balazs J.; Taylor, Wayne Allen; ...

2016-06-04

Here, this paper discusses the development of a separation method for isolation of Tm-171 from a half-gram irradiated erbium target in support of stockpile stewardship and astrophysics research. The developed procedure is based on cation exchange separation using alpha-hydroxyisobutyric acid (α-HIBA) as chelating agent. It is able to achieve either a decontamination factor of 1.4(4) × 10 5 with 68.9(3) % recovery or 95.4(3) % recovery with a decontamination factor of 5.82(7) × 10 3 for a mock 500-mg target containing 17.9 mg thulium in a single pass-through at room temperature.

Development and validation of ultra-high performance supercritical fluid chromatography method for determination of illegal dyes and comparison to ultra-high performance liquid chromatography method.

PubMed

Khalikova, Maria A; Šatínský, Dalibor; Solich, Petr; Nováková, Lucie

2015-05-18

A novel simple, fast and efficient ultra-high performance supercritical fluid chromatography (UHPSFC) method was developed and validated for the separation and quantitative determination of eleven illegal dyes in chili-containing spices. The method involved a simple ultrasound-assisted liquid extraction of illegal compounds with tetrahydrofuran. The separation was performed using a supercritical fluid chromatography system and CSH Fluoro-Phenyl stationary phase at 70°C. The mobile phase was carbon dioxide and the mixture of methanol:acetonitrile (1:1, v/v) with 2.5% formic acid as an additive at the flow rate 2.0 mL min(-1). The UV-vis detection was accomplished at 500 nm for seven compounds and at 420 nm for Sudan Orange G, Butter Yellow, Fast Garnet GBC and Methyl Red due to their maximum of absorbance. All eleven compounds were separated in less than 5 min. The method was successfully validated and applied using three commercial samples of chili-containing spices - Chili sauce (Indonesia), Feferony sauce (Slovakia) and Mojo sauce (Spain). The linearity range of proposed method was 0.50-9.09 mg kg(-1) (r ≥ 0.995). The detection limits were determined as signal to noise ratio of 3 and were ranged from 0.15 mg kg(-1) to 0.60 mg kg(-1) (1.80 mg kg(-1) for Fast Garnet) for standard solution and from 0.25 mg kg(-1) to 1.00 mg kg(-1) (2.50 mg kg(-1) for Fast Garnet, 1.50 mg kg(-1) for Sudan Red 7B) for chili-containing samples. The recovery values were in the range of 73.5-107.2% and relative standard deviation ranging from 0.1% to 8.2% for within-day precision and from 0.5% to 8.8% for between-day precision. The method showed potential for being used to monitor forbidden dyes in food constituents. The developed UHPSFC method was compared to the UHPLC-UV method. The orthogonality of Sudan dyes separation by these two methods was demonstrated. Benefits and drawbacks were discussed showing the reliability of both methods for monitoring of studied illegal dyes in real food constituents. Copyright © 2015 Elsevier B.V. All rights reserved.

Development and validation of LC-MS/MS methods for the determination of mirabegron and its metabolites in human plasma and their application to a clinical pharmacokinetic study.

PubMed

Teijlingen, Raymond van; Meijer, John; Takusagawa, Shin; Gelderen, Marcel van; Beld, Cas van den; Usui, Takashi

2012-03-01

Mirabegron is being developed for the treatment of overactive bladder. To support the development of mirabegron, including pharmacokinetic studies, liquid chromatography/tandem mass spectrometry methods for mirabegron and eight metabolites (M5, M8, M11-M16) were developed and validated for heparinized human plasma containing sodium fluoride. Four separate bioanalytical methods were developed for the analysis of: (1) mirabegron; (2) M5 and M16; (3) M8; and (4) M11-M15. Either solid-phase extraction or liquid-liquid extraction was used to extract the analytes of interest from matrix constituents. For mirabegron, an Inertsil C₈-3 analytical column was used and detection was performed using a triple-quad mass spectrometer equipped with an atmospheric pressure chemical ionization interface. For the metabolite assays, chromatographic separation was performed through a Phenomenex Synergi Fusion-RP C₁₈ analytical column and detection was performed using a triple-quad mass spectrometer equipped with a Heated Electrospray Ionization interface. The validation results demonstrated that the developed liquid chromatography/tandem mass spectrometry methods were precise, accurate, and selective for the determination of mirabegron and its metabolites in human plasma. All methods were successfully applied in evaluating the pharmacokinetic parameters of mirabegron and metabolites in human plasma. Copyright © 2012 Elsevier B.V. All rights reserved.

Novel spectrophotometric methods for simultaneous determination of timolol and dorzolamide in their binary mixture.

PubMed

Lotfy, Hayam Mahmoud; Hegazy, Maha A; Rezk, Mamdouh R; Omran, Yasmin Rostom

2014-05-21

Two smart and novel spectrophotometric methods namely; absorbance subtraction (AS) and amplitude modulation (AM) were developed and validated for the determination of a binary mixture of timolol maleate (TIM) and dorzolamide hydrochloride (DOR) in presence of benzalkonium chloride without prior separation, using unified regression equation. Additionally, simple, specific, accurate and precise spectrophotometric methods manipulating ratio spectra were developed and validated for simultaneous determination of the binary mixture namely; simultaneous ratio subtraction (SRS), ratio difference (RD), ratio subtraction (RS) coupled with extended ratio subtraction (EXRS), constant multiplication method (CM) and mean centering of ratio spectra (MCR). The proposed spectrophotometric procedures do not require any separation steps. Accuracy, precision and linearity ranges of the proposed methods were determined and the specificity was assessed by analyzing synthetic mixtures of both drugs. They were applied to their pharmaceutical formulation and the results obtained were statistically compared to that of a reported spectrophotometric method. The statistical comparison showed that there is no significant difference between the proposed methods and the reported one regarding both accuracy and precision. Copyright © 2014 Elsevier B.V. All rights reserved.

Performances of CN-columns for the analysis of γ-oryzanol and its p-coumarate and caffeate derivatives by normal phase HPLC and a validated method of quantitation.

PubMed

D'Ambrosio, Michele

2013-06-15

γ-Oryzanol is an important phytochemical used in pharmaceutical, alimentary and cosmetic preparations. The present article, for the first time, discloses the performances of NP-HPLC in separating γ-oryzanol components and develops a validated method for its routine quantification. The analysis is performed on a cyanopropyl bonded column using the hexane/MTBE gradient elution and UV detection at 325 nm. The method allows: the separation of steryl ferulate, p-coumarate and caffeate esters, the separation of cis- from trans-ferulate isomers, the splitting of steroid moieties into saturated and unsaturated at the side chain. The optimised method provides excellent linear response (R(2)=0.99997), high precision (RSD<1.0%) and satisfactory accuracy (R(∗)=70-86%). In conclusion, the established method presents the details of the procedure and the experimental conditions in order to achieve the required precision and instrumental accuracy. The method is fast and sensitive and it could be a suitable tool for quality assurance and determination of origin. Copyright © 2012 Elsevier Ltd. All rights reserved.

New test techniques to evaluate near field effects for supersonic store carriage and separation

NASA Technical Reports Server (NTRS)

Sawyer, Wallace C.; Stallings, Robert L., Jr.; Wilcox, Floyd J., Jr.; Blair, A. B., Jr.; Monta, William J.; Plentovich, Elizabeth B.

1989-01-01

Store separation and store carriage drag studies were conducted. A primary purpose is to develop new experimental methods to evaluate near field effects of store separation and levels of store carriage drag associated with a variety of carriage techniques for different store shapes and arrangements. Flow field measurements consisting of surface pressure distributions and vapor screen photographs are used to analyze the variations of the store separation characteristics with cavity geometry. Store carriage drag measurements representative of tangent, semi-submerged, and internal carriage installations are presented and discussed. Results are included from both fully metric models and models with only metric segments (metric pallets) and the relative merits of the two are discussed. Carriage drag measurements for store installations on an aircraft parent body are compared both with prediction methods and with installations on a generic parent body.

Application of an efficient strategy based on liquid-liquid extraction, high-speed counter-current chromatography, and preparative HPLC for the rapid enrichment, separation, and purification of four anthraquinones from Rheum tanguticum.

PubMed

Chen, Tao; Liu, Yongling; Zou, Denglang; Chen, Chen; You, Jinmao; Zhou, Guoying; Sun, Jing; Li, Yulin

2014-01-01

This study presents an efficient strategy based on liquid-liquid extraction, high-speed counter-current chromatography, and preparative HPLC for the rapid enrichment, separation, and purification of four anthraquinones from Rheum tanguticum. A new solvent system composed of petroleum ether/ethyl acetate/water (4:2:1, v/v/v) was developed for the liquid-liquid extraction of the crude extract from R. tanguticum. As a result, emodin, aloe-emodin, physcion, and chrysophanol were greatly enriched in the organic layer. In addition, an efficient method was successfully established to separate and purify the above anthraquinones by high-speed counter-current chromatography and preparative HPLC. This study supplies a new alternative method for the rapid enrichment, separation, and purification of emodin, aloe-emodin, physcione, and chrysophanol. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

[Separation and identification of bovine lactoferricin by high performance liquid chromatography-matrix-assisted laser desorption/ionization time of flight/ time of flight mass spectrometry].

PubMed

An, Meichen; Liu, Ning

2010-02-01

A high performance liquid chromatography-matrix-assisted laser desorption/ionization time of flight/time of flight mass spectrometry (HPLC-MALDI-TOF/TOF MS) method was developed for the separation and identification of bovine lactoferricin (LfcinB). Bovine lactoferrin was hydrolyzed by pepsin and then separated by ion exchange chromatography and reversed-phase liquid chromatography (RP-LC). The antibacterial activities of the fractions from RP-LC separation were determined and the protein concentration of the fraction with the highest activity was measured, whose sequence was indentified by MALDI-TOF/TOF MS. The relative molecular mass of LfcinB was 3 124.89 and the protein concentration was 18.20 microg/mL. The method of producing LfcinB proposed in this study has fast speed, high accuracy and high resolution.

[The research on separating and extracting overlapping spectral feature lines in LIBS using damped least squares method].

PubMed

Wang, Yin; Zhao, Nan-jing; Liu, Wen-qing; Yu, Yang; Fang, Li; Meng, De-shuo; Hu, Li; Zhang, Da-hai; Ma, Min-jun; Xiao, Xue; Wang, Yu; Liu, Jian-guo

2015-02-01

In recent years, the technology of laser induced breakdown spectroscopy has been developed rapidly. As one kind of new material composition detection technology, laser induced breakdown spectroscopy can simultaneously detect multi elements fast and simply without any complex sample preparation and realize field, in-situ material composition detection of the sample to be tested. This kind of technology is very promising in many fields. It is very important to separate, fit and extract spectral feature lines in laser induced breakdown spectroscopy, which is the cornerstone of spectral feature recognition and subsequent elements concentrations inversion research. In order to realize effective separation, fitting and extraction of spectral feature lines in laser induced breakdown spectroscopy, the original parameters for spectral lines fitting before iteration were analyzed and determined. The spectral feature line of' chromium (Cr I : 427.480 nm) in fly ash gathered from a coal-fired power station, which was overlapped with another line(FeI: 427.176 nm), was separated from the other one and extracted by using damped least squares method. Based on Gauss-Newton iteration, damped least squares method adds damping factor to step and adjust step length dynamically according to the feedback information after each iteration, in order to prevent the iteration from diverging and make sure that the iteration could converge fast. Damped least squares method helps to obtain better results of separating, fitting and extracting spectral feature lines and give more accurate intensity values of these spectral feature lines: The spectral feature lines of chromium in samples which contain different concentrations of chromium were separated and extracted. And then, the intensity values of corresponding spectral lines were given by using damped least squares method and least squares method separately. The calibration curves were plotted, which showed the relationship between spectral line intensity values and chromium concentrations in different samples. And then their respective linear correlations were compared. The experimental results showed that the linear correlation of the intensity values of spectral feature lines and the concentrations of chromium in different samples, which was obtained by damped least squares method, was better than that one obtained by least squares method. And therefore, damped least squares method was stable, reliable and suitable for separating, fitting and extracting spectral feature lines in laser induced breakdown spectroscopy.

Separation of alpha-, beta-, gamma-, delta-tocopherols and alpha-tocopherol acetate on a pentaerythritol diacrylate monostearate-ethylene dimethacrylate monolith by capillary electrochromatography.

PubMed

Chaisuwan, Patcharin; Nacapricha, Duangjai; Wilairat, Prapin; Jiang, Zhengjin; Smith, Norman W

2008-06-01

This work reports the first use of a monolith with method development for the separation of tocopherol (TOH) compounds by CEC with UV detection. A pentaerythritol diacrylate monostearate-ethylene dimethacrylate (PEDAS-EDMA) monolithic column has been investigated for an optimised condition to separate alpha-, beta-, gamma- and delta-TOHs, and alpha-tocopherol acetate (TAc). The PEDAS-EDMA monolith showed a remarkably good selectivity for separation of the TOH isomers including the beta- and gamma-isomers which are not easily separated by standard C8 or C18 particle-packed columns. Retention studies indicated that an RP mechanism was involved in the separation on the PEDAS-EDMA column, but polar interactions with the underlying ester and hydroxyl groups enhanced the separation of the problematic beta- and gamma-isomers. Separation of all the compounds was achieved within 25 min using 3:10:87 v/v/v 100 mM Tris buffer (pH 9.3)/methanol/ACN as the mobile phase. The method was successfully applied to a pharmaceutical sample with recoveries from 93 to 99%. Intraday and interday precisions (%RSD) for peak area and retention time were less than 2.3. LODs for all four TOHs and TAc were below 1 ppm.

Predictive framework for shape-selective separations in three-dimensional zeolites and metal-organic frameworks.

PubMed

First, Eric L; Gounaris, Chrysanthos E; Floudas, Christodoulos A

2013-05-07

With the growing number of zeolites and metal-organic frameworks (MOFs) available, computational methods are needed to screen databases of structures to identify those most suitable for applications of interest. We have developed novel methods based on mathematical optimization to predict the shape selectivity of zeolites and MOFs in three dimensions by considering the energy costs of transport through possible pathways. Our approach is applied to databases of over 1800 microporous materials including zeolites, MOFs, zeolitic imidazolate frameworks, and hypothetical MOFs. New materials are identified for applications in gas separations (CO2/N2, CO2/CH4, and CO2/H2), air separation (O2/N2), and chemicals (propane/propylene, ethane/ethylene, styrene/ethylbenzene, and xylenes).

Determination of noscapine, hexylresorcinol and anethole in cough lozenges by liquid chromatography.

PubMed

Lucangioli, S; Fernández Otero, G; Rodríguez, V; Carducci, C N

1996-06-01

A liquid chromatographic method was developed for the simultaneous separation and determination of noscapine hydrochloride, hexylresorcinol and anethole in cough lozenges. Analysis was performed on a phenyl column with phosphate buffer- acetonitrile as mobile phase and the separated components were detected at 282 mm. Recoveries obtained for the analytes were of 94.6% for noscapine hydrochloride, 99.1% for hexylresorcinol and 96.3% for anethole. The values of the relative standard deviation were 0.8% for noscapine hydrochloride, 1.5% for hexylresorcinol and 1.1% for anethole. The analytical method was validated and a system suitability test was accomplished for the chromatographic method.

Optical method for distance and displacement measurements of the probe-sample separation in a scanning near-field optical microscope

DOE Office of Scientific and Technical Information (OSTI.GOV)

Santamaria, L.; Siller, H. R.; Garcia-Ortiz, C. E., E-mail: cegarcia@cicese.mx

In this work, we present an alternative optical method to determine the probe-sample separation distance in a scanning near-field optical microscope. The experimental method is based in a Lloyd’s mirror interferometer and offers a measurement precision deviation of ∼100 nm using digital image processing and numerical analysis. The technique can also be strategically combined with the characterization of piezoelectric actuators and stability evaluation of the optical system. It also opens the possibility for the development of an automatic approximation control system valid for probe-sample distances from 5 to 500 μm.

A thin film degradation study of a fluorinated polyether liquid lubricant using an HPLC method

NASA Technical Reports Server (NTRS)

Morales, W.

1986-01-01

A High Pressure Liquid Chromatography (HPLC) separation method was developed to study and analyze a fluorinated polyether fluid which is promising liquid lubricant for future applications. This HPLC separation method was used in a preliminary study investigating the catalytic effect of various metal, metal alloy, and ceramic engineering materials on the degradation of this fluid in a dry air atmosphere at 345 C. Using a 440 C stainless steel as a reference catalytic material it was found that a titanium alloy and a chromium plated material degraded the fluorinated polyether fluid substantially more than the reference material.

Separation of 2-aminobenzoic acid-derivatized glycosaminoglycans and asparagine-linked glycans by capillary electrophoresis.

PubMed

Sato, Kae; Sato, Kiichi; Okubo, Akira; Yamazaki, Sunao

2005-01-01

A capillary electrophoresis method was developed for the analysis of oligosaccharides combined with derivatization with 2-aminobenzoic acid. Glycosaminoglycan delta-disaccharides were effectively resolved on a fused-silica capillary tube using 150 mM borate, pH 8.5, as a running electrolyte solution. This analytical method was applied to the identification of glycosaminoglycan in combination with enzymatic digestion. The separation of N-glycans or glucose-oligomers was performed with a phosphate buffer containing polyethylene glycol or borate as an electrolyte solution. This method is expected to be useful in the determination of oligosaccharide structures in a glycoprotein.

Recent Developments of Graphene Oxide-Based Membranes: A Review

PubMed Central

Ma, Jinxia; Ping, Dan; Dong, Xinfa

2017-01-01

Membrane-based separation technology has attracted great interest in many separation fields due to its advantages of easy-operation, energy-efficiency, easy scale-up, and environmental friendliness. The development of novel membrane materials and membrane structures is an urgent demand to promote membrane-based separation technology. Graphene oxide (GO), as an emerging star nano-building material, has showed great potential in the membrane-based separation field. In this review paper, the latest research progress in GO-based membranes focused on adjusting membrane structure and enhancing their mechanical strength as well as structural stability in aqueous environment is highlighted and discussed in detail. First, we briefly reviewed the preparation and characterization of GO. Then, the preparation method, characterization, and type of GO-based membrane are summarized. Finally, the advancements of GO-based membrane in adjusting membrane structure and enhancing their mechanical strength, as well as structural stability in aqueous environment, are particularly discussed. This review hopefully provides a new avenue for the innovative developments of GO-based membrane in various membrane applications. PMID:28895877

Recent Developments of Graphene Oxide-Based Membranes: A Review.

PubMed

Ma, Jinxia; Ping, Dan; Dong, Xinfa

2017-09-12

Membrane-based separation technology has attracted great interest in many separation fields due to its advantages of easy-operation, energy-efficiency, easy scale-up, and environmental friendliness. The development of novel membrane materials and membrane structures is an urgent demand to promote membrane-based separation technology. Graphene oxide (GO), as an emerging star nano-building material, has showed great potential in the membrane-based separation field. In this review paper, the latest research progress in GO-based membranes focused on adjusting membrane structure and enhancing their mechanical strength as well as structural stability in aqueous environment is highlighted and discussed in detail. First, we briefly reviewed the preparation and characterization of GO. Then, the preparation method, characterization, and type of GO-based membrane are summarized. Finally, the advancements of GO-based membrane in adjusting membrane structure and enhancing their mechanical strength, as well as structural stability in aqueous environment, are particularly discussed. This review hopefully provides a new avenue for the innovative developments of GO-based membrane in various membrane applications.

Development of a fractionation method for the detection and identification of oak ellagitannins in red wines.

PubMed

García-Estévez, Ignacio; Escribano-Bailón, M Teresa; Rivas-Gonzalo, Julián C; Alcalde-Eon, Cristina

2010-02-15

During maturation and ageing in oak barrels wines improve their organoleptic properties. Ellagitannins can be released from wood to the wine and be involved in oxidation reactions and seem to influence the astringency and colour properties of the wine. Nevertheless, the ellagitannins levels are lower than those of other wine constituents and, consequently, they are not easily detected. This study has developed a two-step fractionation method consisting of a solid phase extraction in C-18 Sep-Pak cartridges followed by size exclusion chromatography in hand-packed Sephadex LH-20 minicolumn for the detection of oak ellagitannins in different types of wines. An HPLC method has also been developed which allows the separation of compounds with the same m/z ratios, facilitating the ellagitannin identification by means of the mass spectrometric analyses. The main oak ellagitannins (grandinin, vescalagin, roburin E and castalagin) were isolated, detected separately and identified in a spiked wine and in three real ones, proving the usefulness of the fractionation method. Copyright 2009 Elsevier B.V. All rights reserved.

Development of a nucleotide sugar purification method using a mixed mode column & mass spectrometry detection.

PubMed

Eastwood, Heather; Xia, Fang; Lo, Mei-Chu; Zhou, Jing; Jordan, John B; McCarter, John; Barnhart, Wesley W; Gahm, Kyung-Hyun

2015-11-10

Analysis of nucleotide sugars, nucleoside di- and triphosphates and sugar-phosphates is an essential step in the process of understanding enzymatic pathways. A facile and rapid separation method was developed to analyze these compounds present in an enzymatic reaction mixture utilized to produce nucleotide sugars. The Primesep SB column explored in this study utilizes hydrophobic interactions as well as electrostatic interactions with the phosphoric portion of the nucleotide sugars. Ammonium formate buffer was selected due to its compatibility with mass spectrometry. Negative ion mode mass spectrometry was adopted for detection of the sugar phosphate (fucose-1-phophate), as the compound is not amenable to UV detection. Various mobile phase conditions such as pH, buffer concentration and organic modifier were explored. The semi-preparative separation method was developed to prepare 30mg of the nucleotide sugar. (19)F NMR was utilized to determine purity of the purified fluorinated nucleotide sugar. The collected nucleotide sugar was found to be 99% pure. Published by Elsevier B.V.

Determination of ambroxol hydrochloride, methylparaben and benzoic acid in pharmaceutical preparations based on sequential injection technique coupled with monolithic column.

PubMed

Satínský, Dalibor; Huclová, Jitka; Ferreira, Raquel L C; Montenegro, Maria Conceição B S M; Solich, Petr

2006-02-13

The porous monolithic columns show high performance at relatively low pressure. The coupling of short monoliths with sequential injection technique (SIA) results in a new approach to implementation of separation step to non-separation low-pressure method. In this contribution, a new separation method for simultaneous determination of ambroxol, methylparaben and benzoic acid was developed based on a novel reversed-phase sequential injection chromatography (SIC) technique with UV detection. A Chromolith SpeedROD RP-18e, 50-4.6 mm column with 10 mm precolumn and a FIAlab 3000 system with a six-port selection valve and 5 ml syringe were used for sequential injection chromatographic separations in our study. The mobile phase used was acetonitrile-tetrahydrofuran-0.05M acetic acid (10:10:90, v/v/v), pH 3.75 adjusted with triethylamine, flow rate 0.48 mlmin(-1), UV-detection was at 245 nm. The analysis time was <11 min. A new SIC method was validated and compared with HPLC. The method was found to be useful for the routine analysis of the active compounds ambroxol and preservatives (methylparaben or benzoic acid) in various pharmaceutical syrups and drops.

[Study of purity tests for silicone resins].

PubMed

Sato, Kyoko; Otsuki, Noriko; Ohori, Akio; Chinda, Mitsuru; Furusho, Noriko; Osako, Tsutomu; Akiyama, Hiroshi; Kawamura, Yoko

2012-01-01

In the 8th edition of Japan's Specifications and Standards for Food Additives, the purity test for silicone resins requires the determination of the refractive index and kinetic viscosity of the extracted silicone oil, and allows for only a limited amount of silicon dioxide. In the purity test, carbon tetrachloride is used to separate the silicone oil and silicon dioxide. To exclude carbon tetrachloride, methods were developed for separating the silicone oil and silicon dioxide from silicone resin, which use hexane and 10% n-dodecylbenzenesulfonic acid in hexane. For silicone oil, the measured refractive index and kinetic viscosity of the silicone oil obtained from the hexane extract were shown to be equivalent to those of the intact silicone oil. In regard to silicon dioxide, it was confirmed that, following the separation with 10% n-dodecylbenzenesulfonic acid in hexane, the level of silicon dioxide in silicone resin can be accurately determined. Therefore, in this study, we developed a method for testing the purity of silicone resins without the use of carbon tetrachloride, which is a harmful reagent.

Unbiased nonorthogonal bases for tomographic reconstruction

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sainz, Isabel; Klimov, Andrei B.; Roa, Luis

2010-05-15

We have developed a general method for constructing a set of nonorthogonal bases with equal separations between all different basis states in prime dimensions. The results are that the corresponding biorthogonal counterparts are pairwise unbiased with the components of the original bases. Using these bases, we derive an explicit expression for the optimal tomography in nonorthogonal bases. A special two-dimensional case is analyzed separately.

Using High Performance Computing to Examine the Processes of Neurogenesis Underlying Pattern Separation/Completion of Episodic Information.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Aimone, James Bradley; Betty, Rita

Using High Performance Computing to Examine the Processes of Neurogenesis Underlying Pattern Separation/Completion of Episodic Information - Sandia researchers developed novel methods and metrics for studying the computational function of neurogenesis, thus generating substantial impact to the neuroscience and neural computing communities. This work could benefit applications in machine learning and other analysis activities.

Development and validation of a simple and robust method for arsenic speciation in human urine using HPLC/ICP-MS.

PubMed

Sen, Indranil; Zou, Wei; Alvaran, Josephine; Nguyen, Linda; Gajek, Ryszard; She, Jianwen

2015-01-01

In order to better distinguish the different toxic inorganic and organic forms of arsenic (As) exposure in individuals, we have developed and validated a simple and robust analytical method for determining the following six As species in human urine: arsenous (III) acid (As-III), As (V) acid, monomethylarsonic acid, dimethylarsinic acid, arsenobetaine (AsB), and arsenocholine. In this method, human urine is diluted using a pH 5.8 buffer, separation is performed using an anion exchange column with isocratic HPLC, and detection is achieved using inductively coupled plasma-MS. The method uses a single mobile phase consisting of low concentrations of both phosphate buffer (5 mM) and ammonium nitrate salt (5 mM) at pH 9.0; this minimizes the column equilibration time and overcomes challenges with separation between AsB and As-III. In addition, As-III oxidation is prevented by degassing the sample preparation buffer at pH 5.8, degassing the mobile phase online at pH 9.0, and by the use of low temperature (-70 °C) and flip-cap airtight tubes for long term storage of samples. The method was validated using externally provided reference samples. Results were in agreement with target values at varying concentrations and successfully passed external performance test criteria. Internal QC samples were prepared and repeatedly analyzed to assess the method's long-term precision, and further analyses were completed on anonymous donor urine to assess the quality of the method's baseline separation. Results from analyses of external reference samples agreed with target values at varying concentrations, and results from precision studies yielded absolute CV values of 3-14% and recovery from 82 to 115% for the six As species. Analysis of anonymous donor urine confirmed the well-resolved baseline separation capabilities of the method for real participant samples.

Isolation of purified oocyst walls and sporocysts from Toxoplasma gondii.

PubMed

Everson, William V; Ware, Michael W; Dubey, J P; Lindquist, H D Alan

2002-01-01

Toxoplasma gondii oocysts are environmentally resistant and can infect virtually all warm-blooded hosts, including humans and livestock. Little is known about the biochemical basis for this resistance of oocysts, and mechanism for excystation of T. gondii sporozoites. The objective of the present study was to evaluate different methods (mechanical fragmentation, gradients, flow cytometry) to separate and purify T. gondii oocyst walls and sporocysts. Oocyst walls were successfully separated and purified using iodixanol gradients. Sporocysts were successfully separated and purified using iodixanol and Percoll gradients. Purification was also achieved by flow cytometry. Flow cytometry with fluorescence-activated cell sorting (FACS) yielded analytical quantities of oocyst walls and intact sporocysts. Flow cytometry with FACS also proved useful for quantitation of purity obtained following iodixanol gradient fractionation. Methods reported in this paper will be useful for analytical purposes, such as proteomic analysis of components unique to this life cycle stage, development of detection methods, or excystation studies.

On-line concentration and determination of all-trans- and 13-cis- retinoic acids in rabbit serum by application of sweeping technique in micellar electrokinetic chromatography.

PubMed

Zhao, Yongxi; Kong, Yu; Wang, Bo; Wu, Yayan; Wu, Hong

2007-03-30

A simple and rapid micellar electrokinetic chromatography (MEKC) method with UV detection was developed for the simultaneous separation and determination of all-trans- and 13-cis-retinoic acids in rabbit serum by on-line sweeping concentration technique. The serum sample was simply deproteinized and centrifuged. Various parameters affecting sample enrichment and separation were systematically investigated. Under optimal conditions, the analytes could be well separated within 17min, and the relative standard deviations (RSD) of migration times and peak areas were less than 3.4%. Compared with the conventional MEKC injection method, the 18- and 19-fold improvements in sensitivity were achieved, respectively. The proposed method has been successfully applied to the determination of all-trans- and 13-cis-retinoic acids in serum samples from rabbits and could be feasible for the further pharmacokinetics study of all-trans-retinoic acid.

Preparation of a dual-enzyme co-immobilized capillary microreactor and simultaneous screening of multiple enzyme inhibitors by capillary electrophoresis.

PubMed

Lin, Pingtan; Zhao, Shulin; Lu, Xin; Ye, Fanggui; Wang, Hengshan

2013-08-01

A CE method based on a dual-enzyme co-immobilized capillary microreactor was developed for the simultaneous screening of multiple enzyme inhibitors. The capillary microreactor was prepared by co-immobilizing adenosine deaminase and xanthine oxidase on the inner wall at the inlet end of the separation capillary. The enzymes were first immobilized on gold nanoparticles, and the functionalized gold nanoparticles were then assembled on the inner wall at the inlet end of the separation capillary treated with polyethyleneimine. With the developed CE method, the substrates and products were baseline separated within 3 min. The activity of the immobilized enzyme can be directly detected by measuring the peak height of the products. A statistical parameter Z' factor was recommended for evaluation of the accuracy of a drug screening system. In the present study, it was calculated to be larger than 0.5, implying a good accuracy. Finally, screening a small compound library containing two known enzyme inhibitors and 20 natural extracts by the proposed method was demonstrated. The known inhibitors were identified, and some natural extracts were found to be positive for two-enzyme inhibition by the present method. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Quantification of the level of fat-soluble vitamins in feed based on the novel microemulsion electrokinetic chromatography (MEEKC) method.

PubMed

Olędzka, Ilona; Kowalski, Piotr; Bałuch, Alicja; Bączek, Tomasz; Paradziej-Łukowicz, Jolanta; Taciak, Marcin; Pastuszewska, Barbara

2014-02-01

Simultaneous quantification of liposoluble vitamins is not a new area of interest, since these compounds co-determine the nutritional quality of food and feed, a field widely explored in the human and animal diet. However, the development of appropriate methods is still a matter of concern, especially when the vitamin composition is highly complex, as is the case with feed designated for laboratory animals, representing a higher health and microbiological status. A method combining microemulsion electrokinetic chromatography (MEEKC) with liquid-liquid extraction was developed for the determination of four fat-soluble vitamins in animal feed. A separation medium consisting of 25 mmol L⁻¹ phosphate buffer (pH 2.5), 2-propanol, 1-butanol, sodium dodecyl sulfate and octane allowed the simultaneous determination of vitamins A, D, E and K within a reasonable time of 25 min. The polarity of the separation voltage was reversed in view of the strongly suppressed electro-osmotic flow, and the applied voltage was set at 12 kV. The fat-soluble vitamins were separated in the order of decreasing hydrophobicity. It was proved that the proposed MEEKC method was sufficiently specific and sensitive for screening fat-soluble vitamins in animal feed samples after their sterilization. © 2013 Society of Chemical Industry.

Use of fluorescent ANTS to examine the BBB-permeability of polysaccharide

PubMed Central

Christopher, Kevin; Makani, Vishruti; Judy, Wesley; Lee, Erica; Chiaia, Nicolas; Kim, Dong Shik; Park, Joshua

2015-01-01

Recently, some polysaccharides showed therapeutic potentials for the treatment of neurodegenerative diseases while the most important property, their permeability to the blood brain barrier (BBB) that sheathes the brain and spinal cord, is not yet determined. The determination has been delayed by the difficulty in tracking a target polysaccharide among endogenous polysaccharides in animal. We developed an easy way to examine the BBB-permeability and, possibly, tissue distribution of a target polysaccharide in animal. We tagged a polysaccharide with fluorescent 8-aminonaphthalene-1,3,6-trisulfonic acid disodium salt (ANTS) for tracking. We also developed a simple method to separate ANTS-tagged polysaccharide from unconjugated free ANTS using 75% ethanol. After ANTS-polysaccharide was intra-nasally administered into animals, we could quantify the amounts of ANTS-polysaccharide in the brain and the serum by fluorocytometry. We could also separate free ANTS-polysaccharide from serum proteins using trichloroacetic acid (TCA) and 75% ethanol. Our method will help to track a polysaccharide in animal easily. • ANTS-labeling is less tedious than but as powerful as radiolabeling for tracking a target polysaccharide in animal. • Our simple method can separate structurally intact ANTS-polysaccharide from animal serum and tissues. • This method is good for the fluorometry-based measurement of ANTS-conjugated macromolecules in tissues. PMID:25914873

Theoretical study of hull-rotor aerodynamic interference on semibuoyant vehicles

NASA Technical Reports Server (NTRS)

Spangler, S. B.; Smith, C. A.

1978-01-01

Analytical methods are developed to predict the pressure distribution and overall loads on the hulls of airships which have close coupled, relatively large and/or high disk loading propulsors for attitude control, station keeping, and partial support of total weight as well as provision of thrust in cruise. The methods comprise a surface-singularity, potential-flow model for the hull and lifting surfaces (such as tails) and a rotor model which calculates the velocity induced by the rotor and its wake at points adjacent to the wake. Use of these two models provides an inviscid pressure distribution on the hull with rotor interference. A boundary layer separation prediction method is used to locate separation on the hull, and a wake pressure is imposed on the separated region for purposes of calculating hull loads. Results of calculations are shown to illustrate various cases of rotor-hull interference and comparisons with small scale data are made to evaluate the method.

Measurement of free carnitine and acylcarnitines in plasma by HILIC-ESI-MS/MS without derivatization.

PubMed

Peng, Minzhi; Liu, Li; Jiang, Minyan; Liang, Cuili; Zhao, Xiaoyuan; Cai, Yanna; Sheng, Huiying; Ou, Zhiying; Luo, Hong

2013-08-01

Measurement of carnitine and acylcarnitines in plasma is important in diagnosis of fatty acid β-oxidation disorders and organic acidemia. The usual method uses flow injection tandem mass spectrometry (FIA-MS/MS), which has limitations. A rapid and more accurate method was developed to be used for high-risk screening and diagnosis. Carnitine and acylcarnitines were separated by hydrophilic interaction liquid chromatography (HILIC) without derivatization and detected with a QTRAP MS/MS System. Total analysis time was 9.0min. The imprecision of within- and between-run were less than 6% and 17%, respectively. Recoveries were in the range of 85-110% at three concentrations. Some acylcarnitine isomers could be separated, such as dicarboxylic and hydroxyl acylcarnitines. The method could also separate interferent to avoid false positive results. 216 normal samples and 116 patient samples were detected with the validated method, and 49 patients were identified with fatty acid oxidation disorders or organic acidemias. Copyright © 2013 Elsevier B.V. All rights reserved.

Development and Validation of a HPTLC Method for Simultaneous Estimation of L-Glutamic Acid and γ-Aminobutyric Acid in Mice Brain

PubMed Central

Sancheti, J. S.; Shaikh, M. F.; Khatwani, P. F.; Kulkarni, Savita R.; Sathaye, Sadhana

2013-01-01

A new robust, simple and economic high performance thin layer chromatographic method was developed for simultaneous estimation of L-glutamic acid and γ-amino butyric acid in brain homogenate. The high performance thin layer chromatographic separation of these amino acid was achieved using n-butanol:glacial acetic acid:water (22:3:5 v/v/v) as mobile phase and ninhydrin as a derivatising agent. Quantitation of the method was achieved by densitometric method at 550 nm over the concentration range of 10-100 ng/spot. This method showed good separation of amino acids in the brain homogenate with Rf value of L-glutamic acid and γ-amino butyric acid as 21.67±0.58 and 33.67±0.58, respectively. The limit of detection and limit of quantification for L-glutamic acid was found to be 10 and 20 ng and for γ-amino butyric acid it was 4 and 10 ng, respectively. The method was also validated in terms of accuracy, precision and repeatability. The developed method was found to be precise and accurate with good reproducibility and shows promising applicability for studying pathological status of disease and therapeutic significance of drug treatment. PMID:24591747

Development and Validation of a HPTLC Method for Simultaneous Estimation of L-Glutamic Acid and γ-Aminobutyric Acid in Mice Brain.

PubMed

Sancheti, J S; Shaikh, M F; Khatwani, P F; Kulkarni, Savita R; Sathaye, Sadhana

2013-11-01

A new robust, simple and economic high performance thin layer chromatographic method was developed for simultaneous estimation of L-glutamic acid and γ-amino butyric acid in brain homogenate. The high performance thin layer chromatographic separation of these amino acid was achieved using n-butanol:glacial acetic acid:water (22:3:5 v/v/v) as mobile phase and ninhydrin as a derivatising agent. Quantitation of the method was achieved by densitometric method at 550 nm over the concentration range of 10-100 ng/spot. This method showed good separation of amino acids in the brain homogenate with Rf value of L-glutamic acid and γ-amino butyric acid as 21.67±0.58 and 33.67±0.58, respectively. The limit of detection and limit of quantification for L-glutamic acid was found to be 10 and 20 ng and for γ-amino butyric acid it was 4 and 10 ng, respectively. The method was also validated in terms of accuracy, precision and repeatability. The developed method was found to be precise and accurate with good reproducibility and shows promising applicability for studying pathological status of disease and therapeutic significance of drug treatment.

A simple method for the analysis of particle sizes of forage and total mixed rations.

PubMed

Lammers, B P; Buckmaster, D R; Heinrichs, A J

1996-05-01

A simple separator was developed to determine the particle sizes of forage and TMR that allows for easy separation of wet forage into three fractions and also allows plotting of the particle size distribution. The device was designed to mimic the laboratory-scale separator for forage particle sizes that was specified by Standard S424 of the American Society of Agricultural Engineers. A comparison of results using the standard device and the newly developed separator indicated no difference in ability to predict fractions of particles with maximum length of less than 8 and 19 mm. The separator requires a small quantity of sample (1.4 L) and is manually operated. The materials on the screens and bottom pan were weighed to obtain the cumulative percentage of sample that was undersize for the two fractions. The results were then plotted using the Weibull distribution, which proved to be the best fit for the data. Convenience samples of haycrop silage, corn silage, and TMR from farms in the northeastern US were analyzed using the forage and TMR separator, and the range of observed values are given.

New technology for separating resin powder and fiberglass powder from fiberglass-resin powder of waste printed circuit boards.

PubMed

Li, Jia; Gao, Bei; Xu, Zhenming

2014-05-06

New recycling technologies have been developed lately to enhance the value of the fiberglass powder-resin powder fraction (FRP) from waste printed circuit boards. The definite aim of the present paper is to present some novel methods that use the image forces for the separation of the resin powder and fiberglass powder generated from FRP during the corona electrostatic separating process. The particle shape charactization and particle trajectory simulation were performed on samples of mixed non-metallic particles. The simulation results pointed out that particles of resin powder and particles of fiberglass powder had different detach trajectories at the conditions of the same size and certain device parameters. An experiment carried out using a corona electrostatic separator validated the possibility of sorting these particles based on the differences in their shape characteristics. The differences in the physical properties of the different types of particles provided the technical basis for the development of electrostatic separation technologies for the recycling industry.

Synthesis and evaluation of a maltose-bonded silica gel stationary phase for hydrophilic interaction chromatography and its application in Ginkgo Biloba extract separation in two-dimensional systems.

PubMed

Sheng, Qianying; Yang, Kaiya; Ke, Yanxiong; Liang, Xinmiao; Lan, Minbo

2016-09-01

Maltose covalently bonded to silica was prepared by using carbonyl diimidazole as a cross-linker and employed as a stationary phase for hydrophilic interaction liquid chromatography. The column efficiency and the effect of water content, buffer concentration, and pH value influenced on retention were investigated. The separation or enrichment selectivity was also studied with nucleosides, saccharides, amino acids, peptides, and glycopeptides. The results indicated that the stationary phase processed good separation efficiency and separation selectivity in hydrophilic interaction liquid chromatography mode. Moreover, a two-dimensional hydrophilic interaction liquid chromatography× reversed-phase liquid chromatography method with high orthogonality was developed to analyze the Ginkgo Biloba extract fractions. The development of this two-dimensional chromatographic system would be an effective tool for the separation of complex samples of different polarities and contents. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A New Cluster Analysis-Marker-Controlled Watershed Method for Separating Particles of Granular Soils.

PubMed

Alam, Md Ferdous; Haque, Asadul

2017-10-18

An accurate determination of particle-level fabric of granular soils from tomography data requires a maximum correct separation of particles. The popular marker-controlled watershed separation method is widely used to separate particles. However, the watershed method alone is not capable of producing the maximum separation of particles when subjected to boundary stresses leading to crushing of particles. In this paper, a new separation method, named as Monash Particle Separation Method (MPSM), has been introduced. The new method automatically determines the optimal contrast coefficient based on cluster evaluation framework to produce the maximum accurate separation outcomes. Finally, the particles which could not be separated by the optimal contrast coefficient were separated by integrating cuboid markers generated from the clustering by Gaussian mixture models into the routine watershed method. The MPSM was validated on a uniformly graded sand volume subjected to one-dimensional compression loading up to 32 MPa. It was demonstrated that the MPSM is capable of producing the best possible separation of particles required for the fabric analysis.

Noise source separation of diesel engine by combining binaural sound localization method and blind source separation method

NASA Astrophysics Data System (ADS)

Yao, Jiachi; Xiang, Yang; Qian, Sichong; Li, Shengyang; Wu, Shaowei

2017-11-01

In order to separate and identify the combustion noise and the piston slap noise of a diesel engine, a noise source separation and identification method that combines a binaural sound localization method and blind source separation method is proposed. During a diesel engine noise and vibration test, because a diesel engine has many complex noise sources, a lead covering method was carried out on a diesel engine to isolate other interference noise from the No. 1-5 cylinders. Only the No. 6 cylinder parts were left bare. Two microphones that simulated the human ears were utilized to measure the radiated noise signals 1 m away from the diesel engine. First, a binaural sound localization method was adopted to separate the noise sources that are in different places. Then, for noise sources that are in the same place, a blind source separation method is utilized to further separate and identify the noise sources. Finally, a coherence function method, continuous wavelet time-frequency analysis method, and prior knowledge of the diesel engine are combined to further identify the separation results. The results show that the proposed method can effectively separate and identify the combustion noise and the piston slap noise of a diesel engine. The frequency of the combustion noise and the piston slap noise are respectively concentrated at 4350 Hz and 1988 Hz. Compared with the blind source separation method, the proposed method has superior separation and identification effects, and the separation results have fewer interference components from other noise.

Development and Validation of Chemometric Spectrophotometric Methods for Simultaneous Determination of Simvastatin and Nicotinic Acid in Binary Combinations.

PubMed

Alahmad, Shoeb; Elfatatry, Hamed M; Mabrouk, Mokhtar M; Hammad, Sherin F; Mansour, Fotouh R

2018-01-01

The development and introduction of combined therapy represent a challenge for analysis due to severe overlapping of their UV spectra in case of spectroscopy or the requirement of a long tedious and high cost separation technique in case of chromatography. Quality control laboratories have to develop and validate suitable analytical procedures in order to assay such multi component preparations. New spectrophotometric methods for the simultaneous determination of simvastatin (SIM) and nicotinic acid (NIA) in binary combinations were developed. These methods are based on chemometric treatment of data, the applied chemometric techniques are multivariate methods including classical least squares (CLS), principal component regression (PCR) and partial least squares (PLS). In these techniques, the concentration data matrix were prepared by using the synthetic mixtures containing SIM and NIA dissolved in ethanol. The absorbance data matrix corresponding to the concentration data matrix was obtained by measuring the absorbance at 12 wavelengths in the range 216 - 240 nm at 2 nm intervals in the zero-order. The spectrophotometric procedures do not require any separation step. The accuracy, precision and the linearity ranges of the methods have been determined and validated by analyzing synthetic mixtures containing the studied drugs. Chemometric spectrophotometric methods have been developed in the present study for the simultaneous determination of simvastatin and nicotinic acid in their synthetic binary mixtures and in their mixtures with possible excipients present in tablet dosage form. The validation was performed successfully. The developed methods have been shown to be accurate, linear, precise, and so simple. The developed methods can be used routinely for the determination dosage form. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

Chromatographic Studies of Protein-Based Chiral Separations

PubMed Central

Bi, Cong; Zheng, Xiwei; Azaria, Shiden; Beeram, Sandya; Li, Zhao; Hage, David S.

2016-01-01

The development of separation methods for the analysis and resolution of chiral drugs and solutes has been an area of ongoing interest in pharmaceutical research. The use of proteins as chiral binding agents in high-performance liquid chromatography (HPLC) has been an approach that has received particular attention in such work. This report provides an overview of proteins that have been used as binding agents to create chiral stationary phases (CSPs) and in the use of chromatographic methods to study these materials and protein-based chiral separations. The supports and methods that have been employed to prepare protein-based CSPs will also be discussed and compared. Specific types of CSPs that are considered include those that employ serum transport proteins (e.g., human serum albumin, bovine serum albumin, and alpha1-acid glycoprotein), enzymes (e.g., penicillin G acylase, cellobiohydrolases, and α-chymotrypsin) or other types of proteins (e.g., ovomucoid, antibodies, and avidin or streptavidin). The properties and applications for each type of protein and CSP will also be discussed in terms of their use in chromatography and chiral separations. PMID:28344977

Development and validation of a capillary electrophoresis method for the determination of codeine, diphenhydramine, ephedrine and noscapine in pharmaceuticals.

PubMed

Gomez, María R; Sombra, Lorena; Olsina, Roberto A; Martínez, Luis D; Silva, María F

2005-01-01

The present work describes a simple, accurate and rapid method for the separation and simultaneous determination of codeine, diphenhydramine, ephedrine and noscapine present in cough-cold syrup formulations by capillary zone electrophoresis. Factors affecting the separation were the buffer pH and concentration, applied voltage, and presence of additives. Separations were carried out in less than 10 min with a 20 mM sodium tetraborate buffer, pH 8.50. The carrier electrolyte gave baseline separation with good resolution, great reproducibility and accuracy. Calibration plots were linear over at least three orders of magnitude of analyte concentrations, the lower limits of detection being within the range 0.42-1.33 microg ml(-1). Detection was performed by UV absorbance at wavelengths of 205 and 250 nm. Quantification of the components in actual syrup formulations was calculated against the responses of freshly prepared external standard solutions. The method was validated and met all analysis requirements of quality assurance and quality control. The procedure was fast and reliable and commercial pharmaceuticals could be analyzed without prior sample clean-up procedure.

Development and validation of dissolution study of sustained release dextromethorphan hydrobromide tablets.

PubMed

Rajan, Sekar; Colaco, Socorrina; Ramesh, N; Meyyanathan, Subramania Nainar; Elango, K

2014-02-01

This study describes the development and validation of dissolution tests for sustained release Dextromethorphan hydrobromide tablets using an HPLC method. Chromatographic separation was achieved on a C18 column utilizing 0.5% triethylamine (pH 7.5) and acetonitrile in the ratio of 50:50. The detection wavelength was 280 nm. The method was validated and response was found to be linear in the drug concentration range of 10-80 microg mL(-1). The suitable conditions were clearly decided after testing sink conditions, dissolution medium and agitation intensity. The most excellent dissolution conditions tested, for the Dextromethorphan hydrobromide was applied to appraise the dissolution profiles. The method was validated and response was found to be linear in the drug concentration range of 10-80 microg mL(-1). The method was established to have sufficient intermediate precision as similar separation was achieved on another instrument handled by different operators. Mean Recovery was 101.82%. Intra precisions for three different concentrations were 1.23, 1.10 0.72 and 1.57, 1.69, 0.95 and inter run precisions were % RSD 0.83, 1.36 and 1.57%, respectively. The method was successfully applied for dissolution study of the developed Dextromethorphan hydrobromide tablets.

A NEW HPLC METHOD FOR SEPARATION OF PHYTOPLANKTON PIGMENTS IN NATURAL SAMPLES

EPA Science Inventory

A new high-performance liquid chromatographic (HPLC) method was developed to analyze, in a single run, most polar and non-polar chlorophylls and carotenoids from marine phytoplankton. The method is based on a reverse-phase amide C16 (RP-amide C16) column and an elution gradient o...

A new method to analyze UV stellar occultation data

NASA Astrophysics Data System (ADS)

Evdokimova, D.; Baggio, L.; Montmessin, F.; Belyaev, D.; Bertaux, J.-L.

2017-09-01

In this paper we present a new method of data processing and a classification of different types of stray light at SPICAV UV stellar occultations. The method was developed on a basis of Richardson-Lucy algorithm including: (a) deconvolution process of measured star light and (b) separation of extra emissions registered by the spectrometer.

Method for the determination of chromium in feed matrix by HPLC.

PubMed

Umesh, Balakrishnan; Rajendran, Rajendra Moorthy; Manoharan, Muthu Tamizh

2015-11-01

An improved method for the chromatographic separation and determination of chromium (III) and (VI) [ CRIII AND CRVI: ] in mineral mixtures and feed samples has been developed. The method uses precolumn derivatization using ammonium pyrrolidinedithiocarbamate ( APD: ) followed by reversed-phase liquid chromatography to separate the chromium ions. Both Cr(III) and Cr(VI) species are chelated with ammonium pyrrolidinedithiocarbamate prior to separation by mixing with acetonitrile and 0.5 mmol acetate buffer (pH 4.5). Optimum chromatographic separations were obtained with a polymer-based reversed-phase column (Kinetex, 5 μ, 250 × 4.5 mm, Phenomenex, Torrance, CA) and a mobile phase containing acetonitrile and water (7:3). Both Cr(III) and Cr(VI) ion concentrations were directly determined from the corresponding areas in the chromatogram. The effect of analytical parameters, including pH, concentration of ligand, incubation temperature, and mobile phase, was optimized for both chromium complexes. The range of the procedure was found to be linear for Cr(III) and Cr(VI) concentrations between 0.125 and 4 μg/mL (r² = 0.9926) and 0.1 and 3.0 μg/mL (r² = 0.9983), respectively. Precision was evaluated by replicate analysis in which the percentage relative standard deviation values for chromium complex were found to be below 4.0. The recoveries obtained (85-115%) for both Cr(III) and Cr(VI) complexes indicated the accuracy of the developed method. The degradation products, as well as the excipients, were well resolved from the chromium complex peak in the chromatogram. Finally, the new method proved to be suitable for routine analysis of Cr(III) and Cr(VI) species in raw materials, mineral mixtures, and feed samples. © 2015 Poultry Science Association Inc.

Separating Atmospheric and Surface Contributions in Hyperspectral Imager for the Coastal Ocean (HICO) Scenes using Informed Non-Negative Matrix Factorization

NASA Astrophysics Data System (ADS)

Wright, L.; Coddington, O.; Pilewskie, P.

2016-12-01

Hyperspectral instruments are a growing class of Earth observing sensors designed to improve remote sensing capabilities beyond discrete multi-band sensors by providing tens to hundreds of continuous spectral channels. Improved spectral resolution, range and radiometric accuracy allow the collection of large amounts of spectral data, facilitating thorough characterization of both atmospheric and surface properties. These new instruments require novel approaches for processing imagery and separating surface and atmospheric signals. One approach is numerical source separation, which allows the determination of the underlying physical causes of observed signals. Improved source separation will enable hyperspectral imagery to better address key science questions relevant to climate change, including land-use changes, trends in clouds and atmospheric water vapor, and aerosol characteristics. We developed an Informed Non-negative Matrix Factorization (INMF) method for separating atmospheric and surface sources. INMF offers marked benefits over other commonly employed techniques including non-negativity, which avoids physically impossible results; and adaptability, which tailors the method to hyperspectral source separation. The INMF algorithm is adapted to separate contributions from physically distinct sources using constraints on spectral and spatial variability, and library spectra to improve the initial guess. We also explore methods to produce an initial guess of the spatial separation patterns. Using this INMF algorithm we decompose hyperspectral imagery from the NASA Hyperspectral Imager for the Coastal Ocean (HICO) with a focus on separating surface and atmospheric signal contributions. HICO's coastal ocean focus provides a dataset with a wide range of atmospheric conditions, including high and low aerosol optical thickness and cloud cover, with only minor contributions from the ocean surfaces in order to isolate the contributions of the multiple atmospheric sources.

Supramolecular separation mechanism of pentafluorophenyl column using ibuprofen and omeprazole as markers: LC-MS and simulation study.

PubMed

Hussain, Afzal; AlAjmi, Mohamed F; Ali, Imran

2018-06-01

The pentafluorophenyl (PFP) column is emerging as a new advancement in separation science to analyze a wide range of analytes and, thus, its separation mechanism at supramolecular level is significant. We developed a mechanism for the separation of ibuprofen and omeprazole using different combinations (ranging from 50:50 to 60:40) of water-acetonitrile containing 0.1% formic acid as the mobile phase. The column used was Waters Acquity UPLC HSS PFP (75 × 2.1 mm, 1.8 μm). The reverse order of elution was observed in different combinations of the mobile phases. The docking study indicated hydrogen bonding between ibuprofen and PFP stationary phase (binding energy was -11.30 kJ/mol). Separation at PFP stationary phase is controlled by hydrogen bonding along with π-π interactions. This stationary phase may be used to analyze both aromatic and aliphatic analytes. The developed mechanism will be useful to separate various analytes by considering the possible interactions, leading to saving of energy, time and money. In addition, this work will be highly useful in preparative chromatography where separation is the major problem at a large scale. Moreover, the developed LC-MS-QTOF method may be used to analyze ibuprofen and omeprazole in an unknown sample owing to the low value of detection limits. Copyright © 2018 John Wiley & Sons, Ltd.

Source separation of municipal solid waste: The effects of different separation methods and citizens' inclination-case study of Changsha, China.

PubMed

Chen, Haibin; Yang, Yan; Jiang, Wei; Song, Mengjie; Wang, Ying; Xiang, Tiantian

2017-02-01

A case study on the source separation of municipal solid waste (MSW) was performed in Changsha, the capital city of Hunan Province, China. The objective of this study is to analyze the effects of different separation methods and compare their effects with citizens' attitudes and inclination. An effect evaluation method based on accuracy rate and miscellany rate was proposed to study the performance of different separation methods. A large-scale questionnaire survey was conducted to determine citizens' attitudes and inclination toward source separation. Survey result shows that the vast majority of respondents hold consciously positive attitudes toward participation in source separation. Moreover, the respondents ignore the operability of separation methods and would rather choose the complex separation method involving four or more subclassed categories. For the effects of separation methods, the site experiment result demonstrates that the relatively simple separation method involving two categories (food waste and other waste) achieves the best effect with the highest accuracy rate (83.1%) and the lowest miscellany rate (16.9%) among the proposed experimental alternatives. The outcome reflects the inconsistency between people's environmental awareness and behavior. Such inconsistency and conflict may be attributed to the lack of environmental knowledge. Environmental education is assumed to be a fundamental solution to improve the effect of source separation of MSW in Changsha. Important management tips on source separation, including the reformation of the current pay-as-you-throw (PAYT) system, are presented in this work. A case study on the source separation of municipal solid waste was performed in Changsha. An effect evaluation method based on accuracy rate and miscellany rate was proposed to study the performance of different separation methods. The site experiment result demonstrates that the two-category (food waste and other waste) method achieves the best effect. The inconsistency between people's inclination and the effect of source separation exists. The proposed method can be expanded to other cities to determine the most effective separation method during planning stages or to evaluate the performance of running source separation systems.

Rapid and Efficient Filtration-Based Procedure for Separation and Safe Analysis of CBRN Mixed Samples

PubMed Central

Bentahir, Mostafa; Laduron, Frederic; Irenge, Leonid; Ambroise, Jérôme; Gala, Jean-Luc

2014-01-01

Separating CBRN mixed samples that contain both chemical and biological warfare agents (CB mixed sample) in liquid and solid matrices remains a very challenging issue. Parameters were set up to assess the performance of a simple filtration-based method first optimized on separate C- and B-agents, and then assessed on a model of CB mixed sample. In this model, MS2 bacteriophage, Autographa californica nuclear polyhedrosis baculovirus (AcNPV), Bacillus atrophaeus and Bacillus subtilis spores were used as biological agent simulants whereas ethyl methylphosphonic acid (EMPA) and pinacolyl methylphophonic acid (PMPA) were used as VX and soman (GD) nerve agent surrogates, respectively. Nanoseparation centrifugal devices with various pore size cut-off (30 kD up to 0.45 µm) and three RNA extraction methods (Invisorb, EZ1 and Nuclisens) were compared. RNA (MS2) and DNA (AcNPV) quantification was carried out by means of specific and sensitive quantitative real-time PCRs (qPCR). Liquid chromatography coupled to time-of-flight mass spectrometry (LC/TOFMS) methods was used for quantifying EMPA and PMPA. Culture methods and qPCR demonstrated that membranes with a 30 kD cut-off retain more than 99.99% of biological agents (MS2, AcNPV, Bacillus Atrophaeus and Bacillus subtilis spores) tested separately. A rapid and reliable separation of CB mixed sample models (MS2/PEG-400 and MS2/EMPA/PMPA) contained in simple liquid or complex matrices such as sand and soil was also successfully achieved on a 30 kD filter with more than 99.99% retention of MS2 on the filter membrane, and up to 99% of PEG-400, EMPA and PMPA recovery in the filtrate. The whole separation process turnaround-time (TAT) was less than 10 minutes. The filtration method appears to be rapid, versatile and extremely efficient. The separation method developed in this work constitutes therefore a useful model for further evaluating and comparing additional separation alternative procedures for a safe handling and preparation of CB mixed samples. PMID:24505375

Computational Methods for MOF/Polymer Membranes.

PubMed

Erucar, Ilknur; Keskin, Seda

2016-04-01

Metal-organic framework (MOF)/polymer mixed matrix membranes (MMMs) have received significant interest in the last decade. MOFs are incorporated into polymers to make MMMs that exhibit improved gas permeability and selectivity compared with pure polymer membranes. The fundamental challenge in this area is to choose the appropriate MOF/polymer combinations for a gas separation of interest. Even if a single polymer is considered, there are thousands of MOFs that could potentially be used as fillers in MMMs. As a result, there has been a large demand for computational studies that can accurately predict the gas separation performance of MOF/polymer MMMs prior to experiments. We have developed computational approaches to assess gas separation potentials of MOF/polymer MMMs and used them to identify the most promising MOF/polymer pairs. In this Personal Account, we aim to provide a critical overview of current computational methods for modeling MOF/polymer MMMs. We give our perspective on the background, successes, and failures that led to developments in this area and discuss the opportunities and challenges of using computational methods for MOF/polymer MMMs. © 2016 The Chemical Society of Japan & Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

A new method for quantifying the performance of EEG blind source separation algorithms by referencing a simultaneously recorded ECoG signal.

PubMed

Oosugi, Naoya; Kitajo, Keiichi; Hasegawa, Naomi; Nagasaka, Yasuo; Okanoya, Kazuo; Fujii, Naotaka

2017-09-01

Blind source separation (BSS) algorithms extract neural signals from electroencephalography (EEG) data. However, it is difficult to quantify source separation performance because there is no criterion to dissociate neural signals and noise in EEG signals. This study develops a method for evaluating BSS performance. The idea is neural signals in EEG can be estimated by comparison with simultaneously measured electrocorticography (ECoG). Because the ECoG electrodes cover the majority of the lateral cortical surface and should capture most of the original neural sources in the EEG signals. We measured real EEG and ECoG data and developed an algorithm for evaluating BSS performance. First, EEG signals are separated into EEG components using the BSS algorithm. Second, the EEG components are ranked using the correlation coefficients of the ECoG regression and the components are grouped into subsets based on their ranks. Third, canonical correlation analysis estimates how much information is shared between the subsets of the EEG components and the ECoG signals. We used our algorithm to compare the performance of BSS algorithms (PCA, AMUSE, SOBI, JADE, fastICA) via the EEG and ECoG data of anesthetized nonhuman primates. The results (Best case >JADE = fastICA >AMUSE = SOBI ≥ PCA >random separation) were common to the two subjects. To encourage the further development of better BSS algorithms, our EEG and ECoG data are available on our Web site (http://neurotycho.org/) as a common testing platform. Copyright © 2017 The Author(s). Published by Elsevier Ltd.. All rights reserved.

The numerical calculation of laminar boundary-layer separation

NASA Technical Reports Server (NTRS)

Klineberg, J. M.; Steger, J. L.

1974-01-01

Iterative finite-difference techniques are developed for integrating the boundary-layer equations, without approximation, through a region of reversed flow. The numerical procedures are used to calculate incompressible laminar separated flows and to investigate the conditions for regular behavior at the point of separation. Regular flows are shown to be characterized by an integrable saddle-type singularity that makes it difficult to obtain numerical solutions which pass continuously into the separated region. The singularity is removed and continuous solutions ensured by specifying the wall shear distribution and computing the pressure gradient as part of the solution. Calculated results are presented for several separated flows and the accuracy of the method is verified. A computer program listing and complete solution case are included.

A multi-stage oil-water-separating process design for the sea oil spill recovery robot

NASA Astrophysics Data System (ADS)

Zhang, Min-ge; Wu, Jian-guo; Lin, Xinhua; Wang, Xiao-ming

2018-03-01

Oil spill have the most common pollution to the marine ecological environment. In the late stage of physical method recovery, because of the thin oil and the strong sea breeze, the recovery vessels has low efficiency and high energy consumption. This paper develops a multi-stage oil-water-separating process carried by the sea oil spill recovery robot in severe conditions. This design consists of three separation process, among which both the first and third process adopt corrugated sheets horizontal oil-water separator, while the second is hydraulic rotary breaker. This design also equiptment with rectifier and cyclone separator and other important components. This process has high flexibility and high recovery efficiency. The implement effect is significant.

Distance Learning in Scientific and Professional Fields of Communication (Interdisciplinary Approach)

ERIC Educational Resources Information Center

Skorikova, Tatyana Petrovna; Khromova, Sergey Sergeevich; Dneprovskaya, Natalia Vitalievna

2016-01-01

Modern level of informational technologies development allows the authors of educational courses to decrease their dependence from technical specialists and to independently develop distance-learning courses and their separate online components, which require special methodical learning. The aim of present study is to develop a distance-learning…

On Anticipatory Development of Dual Education Based on the Systemic Approach

ERIC Educational Resources Information Center

Alshynbayeva, Zhuldyz; Sarbassova, Karlygash; Galiyeva, Temir; Kaltayeva, Gulnara; Bekmagambetov, Aidos

2016-01-01

The article addresses separate theoretical and methodical aspects of the anticipatory development of dual education in the Republic of Kazakhstan based on the systemic approach. It states the need to develop orientating basis of prospective professional activities in students. We define the concepts of anticipatory cognition and anticipatory…

In vivo labeling and specific magnetic bead separation of RNA for biofilm characterization and stress-induced gene expression analysis in bacteria.

PubMed

Stankiewicz, Nikolai; Gold, Andrea; Yüksel, Yousra; Berensmeier, Sonja; Schwartz, Thomas

2009-12-01

The method of in vivo labeling and separation of bacterial RNA was developed as an approach to elucidating the stress response of natural bacterial populations. This technique is based on the incorporation of digoxigenin-11-uridine-5'-triphosphate (DIG-11-UTP) in the RNA of active bacteria. The digoxigenin fulfills a dual role as a label of de novo synthesized RNA and a target for magnetic bead separation from a total RNA extract. Depending on the growth conditions and the population's composition, the assembly rate of DIG-11-UTP ranged from 1.2% to 12.5% of the total RNA in gram-positive and gram-negative reference bacteria as well as in natural biofilms from drinking water, surface water, and lake sediment. Separation of DIG-RNA from total RNA extracts was performed with a biotinylated anti-digoxigenin antibody and streptavidin-functionalized magnetic particles. The average separation yield from total RNA extracts was about 95% of labeled RNA. The unspecific bindings of non-labeled nucleic acids were smaller than 0.2%, as was evaluated by spiking experiments with an unmarked DNA amplicon. Applicability of the method developed was demonstrated by rRNA-directed PCR-DGGE population analysis of natural biofilms and expression profiling of two stress-induced genes (vanA and rpoS) in reference bacteria.

Effects of boundary-layer separation controllers on a desktop fume hood.

PubMed

Huang, Rong Fung; Chen, Jia-Kun; Hsu, Ching Min; Hung, Shuo-Fu

2016-10-02

A desktop fume hood installed with an innovative design of flow boundary-layer separation controllers on the leading edges of the side plates, work surface, and corners was developed and characterized for its flow and containment leakage characteristics. The geometric features of the developed desktop fume hood included a rearward offset suction slot, two side plates, two side-plate boundary-layer separation controllers on the leading edges of the side plates, a slanted surface on the leading edge of the work surface, and two small triangular plates on the upper left and right corners of the hood face. The flow characteristics were examined using the laser-assisted smoke flow visualization technique. The containment leakages were measured by the tracer gas (sulphur hexafluoride) detection method on the hood face plane with a mannequin installed in front of the hood. The results of flow visualization showed that the smoke dispersions induced by the boundary-layer separations on the leading edges of the side plates and work surface, as well as the three-dimensional complex flows on the upper-left and -right corners of the hood face, were effectively alleviated by the boundary-layer separation controllers. The results of the tracer gas detection method with a mannequin standing in front of the hood showed that the leakage levels were negligibly small (≤0.003 ppm) at low face velocities (≥0.19 m/s).

Identification and measurement of beta-lactam antibiotic residues in milk: integration of screening kits with liquid chromatography.

PubMed

Harik-Khan, R; Moats, W A

1995-01-01

A procedure for identifying and quantitating violative beta-lactams in milk is described. This procedure integrates beta-lactam residue detection kits with the multiresidue automated liquid chromatographic (LC) cleanup method developed in our laboratory. Spiked milk was deproteinized, extracted, and subjected to reversed-phase LC using a gradient program that concentrated the beta-lactams. Amoxicillin, ampicillin, cephapirin, ceftiofur, cloxacillin, and penicillin G were, thus, separated into 5 fractions that were subsequently tested for activity by using 4 kits. beta-lactams in the positive fractions were quantitated by analytical LC methods developed in our laboratory. The LC cleanup method separated beta-lactam antibiotics from each other and from interferences in the matrix and also concentrated the antibiotics, thus increasing the sensitivity of the kits to the beta-lactam antibiotics. The procedure facilitated the task of identifying and measuring the beta-lactam antibiotics that may be present in milk samples.

Role of chromatography in the development of Standard Reference Materials for organic analysis.

PubMed

Wise, Stephen A; Phinney, Karen W; Sander, Lane C; Schantz, Michele M

2012-10-26

The certification of chemical constituents in natural-matrix Standard Reference Materials (SRMs) at the National Institute of Standards and Technology (NIST) can require the use of two or more independent analytical methods. The independence among the methods is generally achieved by taking advantage of differences in extraction, separation, and detection selectivity. This review describes the development of the independent analytical methods approach at NIST, and its implementation in the measurement of organic constituents such as contaminants in environmental materials, nutrients and marker compounds in food and dietary supplement matrices, and health diagnostic and nutritional assessment markers in human serum. The focus of this review is the important and critical role that separation science techniques play in achieving the necessary independence of the analytical steps in the measurement of trace-level organic constituents in natural matrix SRMs. Published by Elsevier B.V.

Asymmetric organic-inorganic hybrid membrane formation via block copolymer-nanoparticle co-assembly.

PubMed

Gu, Yibei; Dorin, Rachel M; Wiesner, Ulrich

2013-01-01

A facile method for forming asymmetric organic-inorganic hybrid membranes for selective separation applications is developed. This approach combines co-assembly of block copolymer (BCP) and inorganic nanoparticles (NPs) with non-solvent induced phase separation. The method is successfully applied to two distinct molar mass BCPs with different fractions of titanium dioxide (TiO2) NPs. The resulting hybrid membranes exhibit structural asymmetry with a thin nanoporous surface layer on top of a macroporous fingerlike support layer. Key parameters that dictate membrane surface morphology include the fraction of inorganics used and the length of time allowed for surface layer development. The resulting membranes exhibit both good selectivity and high permeability (3200 ± 500 Lm(-2) h(-1) bar(-1)). This fast and straightforward synthesis method for asymmetric hybrid membranes provides a new self-assembly platform upon which multifunctional and high-performance organic-inorganic hybrid membranes can be formed.

High-performance liquid chromatography separation and intact mass analysis of detergent-solubilized integral membrane proteins

PubMed Central

Berridge, Georgina; Chalk, Rod; D’Avanzo, Nazzareno; Dong, Liang; Doyle, Declan; Kim, Jung-In; Xia, Xiaobing; Burgess-Brown, Nicola; deRiso, Antonio; Carpenter, Elisabeth Paula; Gileadi, Opher

2011-01-01

We have developed a method for intact mass analysis of detergent-solubilized and purified integral membrane proteins using liquid chromatography–mass spectrometry (LC–MS) with methanol as the organic mobile phase. Membrane proteins and detergents are separated chromatographically during the isocratic stage of the gradient profile from a 150-mm C3 reversed-phase column. The mass accuracy is comparable to standard methods employed for soluble proteins; the sensitivity is 10-fold lower, requiring 0.2–5 μg of protein. The method is also compatible with our standard LC–MS method used for intact mass analysis of soluble proteins and may therefore be applied on a multiuser instrument or in a high-throughput environment. PMID:21093405

Preparation of water and ice samples for 39Ar dating by atom trap trace analysis (ATTA)

NASA Astrophysics Data System (ADS)

Schwefel, R.; Reichel, T.; Aeschbach-Hertig, W.; Wagenbach, D.

2012-04-01

Atom trap trace analysis (ATTA) is a new and promising method to measure very rare noble gas radioisotopes in the environment. The applicability of this method for the dating of very old groundwater with 81Kr has already been demonstrated [1]. Recent developments now show its feasibility also for the analysis of 39Ar [2,3], which is an ideal dating tracer for the age range between 50 and 1000 years. This range is of interest in the fields of hydro(geo)logy, oceanography, and glaciology. We present preparation (gas extraction and Ar separation) methods for groundwater and ice samples for later analysis by the ATTA technique. For groundwater, the sample size is less of a limitation than for applications in oceanography or glaciology. Large samples are furthermore needed to enable a comparison with the classical method of 39Ar detection by low-level counting. Therefore, a system was built that enables gas extraction from several thousand liters of water using membrane contactors. This system provides degassing efficiencies greater than 80 % and has successfully been tested in the field. Gas samples are further processed to separate a pure Ar fraction by a gas-chromatographic method based on Li-LSX zeolite as selective adsorber material at very low temperatures. The gas separation achieved by this system is controlled by a quadrupole mass spectrometer. It has successfully been tested and used on real samples. The separation efficiency was found to be strongly temperature dependent in the range of -118 to -130 °C. Since ATTA should enable the analysis of 39Ar on samples of less than 1 ccSTP of Ar (corresponding to about 100 ml of air, 2.5 l of water or 1 kg of ice), a method to separate Ar from small amounts of gas was developed. Titanium sponge was found to absorb 60 ccSTP of reactive gases per g of the getter material with reasonably high absorption rates at high operating temperatures (~ 800 ° C). Good separation (higher than 92 % Ar content in residual gas) was achieved by this gettering process. The other main remaining component is H2, which can be further reduced by operating the Ti getter at lower temperature. Furthermore, a system was designed to degas ice samples, followed by Ar separation by gettering. Ice from an alpine glacier was successfully processed on this system.

Distributed-Lagrange-Multiplier-based computational method for particulate flow with collisions

NASA Astrophysics Data System (ADS)

Ardekani, Arezoo; Rangel, Roger

2006-11-01

A Distributed-Lagrange-Multiplier-based computational method is developed for colliding particles in a solid-fluid system. A numerical simulation is conducted in two dimensions using the finite volume method. The entire domain is treated as a fluid but the fluid in the particle domains satisfies a rigidity constraint. We present an efficient method for predicting the collision between particles. In earlier methods, a repulsive force was applied to the particles when their distance was less than a critical value. In this method, an impulsive force is computed. During the frictionless collision process between two particles, linear momentum is conserved while the tangential forces are zero. Thus, instead of satisfying a condition of rigid body motion for each particle separately, as done when particles are not in contact, both particles are rigidified together along their line of centers. Particles separate from each other when the impulsive force is less than zero and after this time, a rigidity constraint is satisfied for each particle separately. Grid independency is implemented to ensure the accuracy of the numerical simulation. A comparison between this method and previous collision strategies is presented and discussed.

Numerical simulation of separated flows. Ph.D. Thesis - Stanford Univ., Calif.

NASA Technical Reports Server (NTRS)

Spalart, P. R.; Leonard, A.; Baganoff, D.

1983-01-01

A new numerical method, based on the Vortex Method, for the simulation of two-dimensional separated flows, was developed and tested on a wide range of gases. The fluid is incompressible and the Reynolds number is high. A rigorous analytical basis for the representation of the Navier-Stokes equation in terms of the vorticity is used. An equation for the control of circulation around each body is included. An inviscid outer flow (computed by the Vortex Method) was coupled with a viscous boundary layer flow (computed by an Eulerian method). This version of the Vortex Method treats bodies of arbitrary shape, and accurately computes the pressure and shear stress at the solid boundary. These two quantities reflect the structure of the boundary layer. Several versions of the method are presented and applied to various problems, most of which have massive separation. Comparison of its results with other results, generally experimental, demonstrates the reliability and the general accuracy of the new method, with little dependence on empirical parameters. Many of the complex features of the flow past a circular cylinder, over a wide range of Reynolds numbers, are correctly reproduced.

Development and Optimization of a Flocculation Procedure for Improved Solid-Liquid Separation of Digested Biomass

DOE Office of Scientific and Technical Information (OSTI.GOV)

Patton, Caroline; Lischeske, James J.; Sievers, David A.

2015-11-03

One viable treatment method for conversion of lignocellulosic biomass to biofuels begins with saccharification (thermochemical pretreatment and enzymatic hydrolysis), followed by fermentation or catalytic upgrading to fuels such as ethanol, butanol, or other hydrocarbons. The post-hydrolysis slurry is typically 4-8 percent insoluble solids, predominantly consisting of lignin. Suspended solids are known to inhibit fermentation as well as poison catalysts and obstruct flow in catalyst beds. Thus a solid-liquid separation following enzymatic hydrolysis would be highly favorable for process economics, however the material is not easily separated by filtration or gravimetric methods. Use of a polyacrylamide flocculant to bind the suspendedmore » particles in a corn stover hydrolyzate slurry into larger flocs (1-2mm diameter) has been found to be extremely helpful in improving separation. Recent and ongoing research on novel pretreatment methods yields hydrolyzate material with diverse characteristics. Therefore, we need a thorough understanding of rapid and successful flocculation design in order to quickly achieve process design goals. In this study potential indicators of flocculation performance were investigated in order to develop a rapid analysis method for flocculation procedure in the context of a novel hydrolyzate material. Flocculation conditions were optimized on flocculant type and loading, pH, and mixing time. Filtration flux of the hydrolyzate slurry was improved 170-fold using a cationic polyacrylamide flocculant with a dosing of approximately 22 mg flocculant/g insoluble solids at an approximate pH of 3. With cake washing, sugar recovery exceeded 90 percent with asymptotic yield at 15 L wash water/kg insoluble solids.« less

Advanced ballistic range technology

NASA Technical Reports Server (NTRS)

Yates, Leslie A.

1994-01-01

The research conducted supported two facilities at NASA Ames Research Center: the Hypervelocity Free-Flight Aerodynamic Facility and the 16-Inch Shock Tunnel. During the grant period, a computerized film-reading system was developed, and five- and six-degree-of-freedom parameter-identification routines were written and successfully implemented. Studies of flow separation were conducted, and methods to extract phase shift information from finite-fringe interferograms were developed. Methods for constructing optical images from Computational Fluid Dynamics solutions were also developed, and these methods were used for one-to-one comparisons of experiment and computations.

Separation of cancer cells from white blood cells by pinched flow fractionation.

PubMed

Pødenphant, Marie; Ashley, Neil; Koprowska, Kamila; Mir, Kalim U; Zalkovskij, Maksim; Bilenberg, Brian; Bodmer, Walter; Kristensen, Anders; Marie, Rodolphe

2015-12-21

In this paper, the microfluidic size-separation technique pinched flow fractionation (PFF) is used to separate cancer cells from white blood cells (WBCs). The cells are separated at efficiencies above 90% for both cell types. Circulating tumor cells (CTCs) are found in the blood of cancer patients and can form new tumors. CTCs are rare cells in blood, but they are important for the understanding of metastasis. There is therefore a high interest in developing a method for the enrichment of CTCs from blood samples, which also enables further analysis of the separated cells. The separation is challenged by the size overlap between cancer cells and the 10(6) times more abundant WBCs. The size overlap prevents high efficiency separation, however we demonstrate that cell deformability can be exploited in PFF devices to gain higher efficiencies than expected from the size distribution of the cells.

Silicon concentrator cell-assembly development

NASA Astrophysics Data System (ADS)

1982-08-01

The purpose was to develop an improved cell assembly design for photovoltaic concentrator receivers. Efforts were concentrated on a study of adhesive/separator systems that might be applied between cell and substrate, because this area holds the key to improved heat transfer, electrical isolation and adhesion. It is also the area in which simpler construction methods offer the greatest benefits for economy and reliability in the manufacturing process. Of the ten most promising designs subjected to rigorous environmental testing, eight designs featuring acrylic and silicon adhesives and fiberglass and polyester separators performed very well.

Systematic reviews: Separating fact from fiction.

PubMed

Haddaway, Neal R; Bilotta, Gary S

2016-01-01

The volume of scientific literature continues to expand and decision-makers are faced with increasingly unmanageable volumes of evidence to assess. Systematic reviews (SRs) are powerful tools that aim to provide comprehensive, transparent, reproducible and updateable summaries of evidence. SR methods were developed, and have been employed, in healthcare for more than two decades, and they are now widely used across a broad range of topics, including environmental management and social interventions in crime and justice, education, international development, and social welfare. Despite these successes and the increasing acceptance of SR methods as a 'gold standard' in evidence-informed policy and practice, misconceptions still remain regarding their applicability. The aim of this article is to separate fact from fiction, addressing twelve common misconceptions that can influence the decision as to whether a SR is the most appropriate method for evidence synthesis for a given topic. Through examples, we illustrate the flexibility of SR methods and demonstrate their suitability for addressing issues on environmental health and chemical risk assessment. Copyright © 2015 Elsevier Ltd. All rights reserved.

Electrophoretic separation techniques and their hyphenation to mass spectrometry in biological inorganic chemistry.

PubMed

Holtkamp, Hannah; Grabmann, Gerlinde; Hartinger, Christian G

2016-04-01

Electrophoretic methods have been widely applied in research on the roles of metal complexes in biological systems. In particular, CE, often hyphenated to a sensitive MS detector, has provided valuable information on the modes of action of metal-based pharmaceuticals, and more recently new methods have been added to the electrophoretic toolbox. The range of applications continues to expand as a result of enhanced CE-to-MS interfacing, with sensitivity often at picomolar level, and evolved separation modes allowing for innovative sample analysis. This article is a followup to previous reviews about CE methods in metallodrug research (Electrophoresis, 2003, 24, 2023-2037; Electrophoresis, 2007, 28, 3436-3446; Electrophoresis, 2012, 33, 622-634), also providing a comprehensive overview of metal species studied by electrophoretic methods hyphenated to MS. It highlights the latest CE developments, takes a sneak peek into gel electrophoresis, traces biomolecule labeling, and focuses on the importance of early-stage drug development. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Velocity gap mode of capillary electrophoresis developed for high-resolution chiral separations.

PubMed

Li, Xue; Li, Youxin; Zhao, Lumeng; Shen, Jianguo; Zhang, Yong; Bao, James J

2014-10-01

A new CE method based on velocity gap (VG) theory has been developed for high-resolution chiral separations. In VG, two consecutive electric fields are adopted to drive analytes passing through two capillaries, which are linked together through a joint. The joint is immersed inside another buffer vial which has conductivity communication with the buffer inside the capillary. By adjusting the field strengths onto the two capillaries, it is possible to observe different velocities of an analyte when it passes through those two capillaries and there would be a net velocity change (NVC) for the same analyte. Different analytes may have different NVC which may be specifically meaningful for enantioseparations because enantiomers are usually hard to resolve. By taking advantage of this NVC, it is possible to enhance the resolution of a chiral separation if a proper voltage program is applied. The feasibility of using NVC to enhance chiral separation was demonstrated in the separations of three pairs of enantiomers: terbutaline, chlorpheniramine, and promethazine. All separations started with partial separation in a conventional CE and were significantly improved under the same experimental conditions. The results indicated that VG has the potential to be used to improve the resolving power of CE in chiral separations. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

SOLVENT EXTRACTION PROCESS FOR SEPARATING URANIUM AND PLUTONIUM FROM AQUEOUS ACIDIC SOLUTIONS OF NEUTRON IRRADIATED URANIUM

DOEpatents

Bruce, F.R.

1962-07-24

A solvent extraction process was developed for separating actinide elements including plutonium and uranium from fission products. By this method the ion content of the acidic aqueous solution is adjusted so that it contains more equivalents of total metal ions than equivalents of nitrate ions. Under these conditions the extractability of fission products is greatly decreased. (AEC)

Lipid-Based Immuno-Magnetic Separation of Archaea from a Mixed Community

NASA Astrophysics Data System (ADS)

Frickle, C. M.; Bailey, J.; Lloyd, K. G.; Shumaker, A.; Flood, B.

2014-12-01

Despite advancing techniques in microbiology, an estimated 98% of all microbial species on Earth have yet to be isolated in pure culture. Natural samples, once transferred to the lab, are commonly overgrown by "weed" species whose metabolic advantages enable them to monopolize available resources. Developing new methods for the isolation of thus-far uncultivable microorganisms would allow us to better understand their ecology, physiology and genetic potential. Physically separating target organisms from a mixed community is one approach that may allow enrichment and growth of the desired strain. Here we report on a novel method that uses known physiological variations between taxa, in this case membrane lipids, to segregate the desired organisms while keeping them alive and viable for reproduction. Magnetic antibodies bound to the molecule squalene, which is found in the cell membranes of certain archaea, but not bacteria, enable separation of archaea from bacteria in mixed samples. Viability of cells was tested by growing the separated fractions in batch culture. Efficacy and optimization of the antibody separation technique are being evaluated using qPCR and cell counts. Future work will apply this new separation technique to natural samples.

Modern separation techniques coupled to high performance mass spectrometry for glycolipid analysis.

PubMed

Sarbu, Mirela; Zamfir, Alina Diana

2018-01-21

Glycolipids (GLs), involved in biological processes and pathologies, such as viral, neurodegenerative and oncogenic transformations are in the focus of research related to method development for structural analysis. This review highlights modern separation techniques coupled to mass spectrometry (MS) for the investigation of GLs from various biological matrices. First section is dedicated to methods, which, although provide the separation in a non-liquid phase, are able to supply important data on the composition of complex mixtures. While classical thin layer chromatography (TLC) is useful for MS analyses of the fractionated samples, ultramodern ion mobility (IMS) characterized by high reproducibility facilitates to discover minor species and to apply low sample amounts, in addition to providing conformational separation with isomer discrimination. Second section highlights the advantages, applications and limitations of liquid-based separation techniques such as high performance liquid chromatography (HPLC) and hydrophilic interaction liquid chromatography (HILIC) in direct or indirect coupling to MS for glycolipidomics surveys. The on- and off-line capillary electrophoresis (CE) MS, offering a remarkable separation efficiency of GLs is also presented and critically assessed from the technical and application perspective in the final part of the review. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Optimization of the Separation of NDA-Derivatized Methylarginines by Capillary and Microchip Electrophoresis

PubMed Central

Linz, Thomas H.; Snyder, Christa M.; Lunte, Susan M.

2013-01-01

The methylated arginines (MAs) monomethylarginine (MMA), asymmetric dimethylarginine (ADMA), and symmetric dimethylarginine (SDMA) have been shown to be independent predictors of cardiovascular disease. This article describes progress regarding the development of an analytical method capable of rapidly analyzing MAs using capillary electrophoresis (CE) and microchip electrophoresis (MCE) with laser-induced fluorescence (LIF) detection. Several parameters including buffer composition and separation voltage were optimized to achieve an ideal separation. The analytes of interest were derivatized with naphthalene-2,3-dicarboxaldehyde (NDA) to produce fluorescent 1-cyanobenz[f]isoindole (CBI) derivatives and then subjected to CE analysis. Baseline resolution of SDMA, ADMA, MMA, and arginine was achieved in less than 8 min. The limits of detection for SDMA, ADMA, MMA, and arginine were determined to be 15, 20, 25, and 5 nM, respectively, which are well below the expected plasma concentrations. The CE separation method was then transferred to a glass MCE device with LIF detection. MAs were baseline resolved in 3 min on-chip using a 14 cm separation channel with detection limits of approximately 10 nM for each species. To the best of the authors’ knowledge, this is the first report of the separation of MAs by MCE. PMID:22357605

Chiral separation of phenylalanine and tryptophan by capillary electrophoresis using a mixture of β-CD and chiral ionic liquid ([TBA] [L-ASP]) as selectors.

PubMed

Yujiao, Wu; Guoyan, Wang; Wenyan, Zhao; Hongfen, Zhang; Huanwang, Jing; Anjia, Chen

2014-05-01

In this paper, a simple, effective and green capillary electrophoresis separation and detection method was developed for the quantification of underivatized amino acids (dl-phenylalanine; dl-tryptophan) using β-Cyclodextrin and chiral ionic liquid ([TBA] [l-ASP]) as selectors. Separation parameters such as buffer concentrations, pH, β-CD and chiral ionic liquid concentrations and separation voltage were investigated for the enantioseparation in order to achieve the maximum possible resolution. A good separation was achieved in a background electrolyte composed of 15 mm sodium tetraborate, 5 mm β-CD and 4 mm chiral ionic liquid at pH 9.5, and an applied voltage of 10 kV. Under optimum conditions, linearity was achieved within concentration ranges from 0.08 to 10 µg/mL for the analytes with correlation coefficients from 0.9956 to 0.9998, and the analytes were separated in less than 6 min with efficiencies up to 970,000 plates/m. The proposed method was successfully applied to the determination of amino acid enantiomers in compound amino acids injections, such as 18AA-I, 18AA-II and 3AA.

Development of Electrospun Nanomaterials and their Applications in Separation Science

NASA Astrophysics Data System (ADS)

Newsome, Toni Elwell

In separations, efficiency is inversely related to the diameter of the sorbent particles of the stationary phase. Thus, materials research in separation science has primarily been directed towards reducing the diameter of the sorbent particle used in the stationary phase. In this dissertation, innovative methods designed for the fabrication and application of electrospun sorbent nanomaterials for separation science are described. Electrospinning is a facile, cost-effective technique that relies on repulsive electrostatic forces to produce nanofibers from a viscoelastic solution. Here, electrospinning is used to generate polymer, carbon, and silica-based nanofibers which are employed as sorbent nanomaterials in extractions and separations. Electrospun carbon nanofibers have proven to be ideal extractive phases for solid-phase microextraction (SPME) when coupled to gas chromatography (GC) for headspace sampling of volatile analytes. Herein, these carbon nanofibers were employed in the direct extraction of nonvolatile analytes and coupled to liquid chromatography (LC) for the first time. The high surface area of the coatings led to enhanced extraction efficiencies; they offered a 3-33 fold increase in efficiency relative to a commercial SPME phase. Carbon nanofibers proved to be stable when immersed in liquids common to LC demonstrating the enhanced stability of these coatings in SPME coupled to LC relative to conventional SPME fibers. The enhanced chemical and mechanical stability of the carbon SPME coatings considerably expanded the range of compounds applicable to SPME and extended the lifetimes of the fibers. Electrospun nanofibers have also proven to be ideal stationary phases in ultra-thin layer chromatography (UTLC). Nanofibers provide faster separations and enhanced separation efficiencies compared to commercial particle-based stationary phases in a relatively short distance. Here, the electrospun-UTLC technology was extended for the first time to nanofibers composed of silica, the most commonly used surface for TLC. An electrospinning method was optimized to produce silica-based nanofibers with the smallest diameter possible (300-380 nm) while maintaining homogenous nanofiber morphology. Highly efficient separations were performed in 15 mm with observed plate heights as low as 8.6 mum. Silica-based nanofibers proved to be chemically stable with a wide variety of TLC reagents demonstrating the enhanced compatibility of these phases with common TLC methods relative to polymer and carbon nanofiber UTLC plates. The extension of electrospun UTLC to silica-based nanofibers vastly expanded the range of analytes and TLC methods which can be used with this technology. The main disadvantage of conventional TLC development methods is that the mobile phase velocity decreases with increasing separation distance. Here, the chromatographic performance of electrospun polymer stationary phases was further improved by using a forced-flow mobile phase in planar electrochromatography (PEC) in which mobile phase velocity does not diminish with increasing distance. Separations were performed on polymer nanofiber UTLC plates in 1-2 min. Compared to UTLC, PEC offered unique selectivity, decreased analysis times (> 4 times faster), and enhanced efficiency (2-3 times lower plate height). In addition, two-dimensional (2D) separations of a complex analyte mixture using UTLC followed by PEC required only 11 min and exhibited a significant increase in separation number (70-77).

A New Cluster Analysis-Marker-Controlled Watershed Method for Separating Particles of Granular Soils

PubMed Central

Alam, Md Ferdous

2017-01-01

An accurate determination of particle-level fabric of granular soils from tomography data requires a maximum correct separation of particles. The popular marker-controlled watershed separation method is widely used to separate particles. However, the watershed method alone is not capable of producing the maximum separation of particles when subjected to boundary stresses leading to crushing of particles. In this paper, a new separation method, named as Monash Particle Separation Method (MPSM), has been introduced. The new method automatically determines the optimal contrast coefficient based on cluster evaluation framework to produce the maximum accurate separation outcomes. Finally, the particles which could not be separated by the optimal contrast coefficient were separated by integrating cuboid markers generated from the clustering by Gaussian mixture models into the routine watershed method. The MPSM was validated on a uniformly graded sand volume subjected to one-dimensional compression loading up to 32 MPa. It was demonstrated that the MPSM is capable of producing the best possible separation of particles required for the fabric analysis. PMID:29057823

Indirect fluorometric detection techniques on thin layer chromatography and effect of ultrasound on gel electrophoresis

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yinfa, Ma.

Thin-layer chromatography (TLC) is a broadly applicable separation technique. It offers many advantages over high performance liquid chromatography (HPLC), such as easily adapted for two-dimensional separation, for whole-column'' detection and for handling multiple samples, etc. However, due to its draggy development of detection techniques comparing with HPLC, TLC has not received the attention it deserves. Therefore, exploring new detection techniques is very important to the development of TLC. It is the principal of this dissertation to present a new detection method for TLC -- indirect fluorometric detection method. This detection technique is universal sensitive, nondestructive, and simple. This will bemore » described in detail from Sections 1 through Section 5. Section 1 and 3 describe the indirect fluorometric detection of anions and nonelectrolytes in TLC. In Section 2, a detection method for cations based on fluorescence quenching of ethidium bromide is presented. In Section 4, a simple and interesting TLC experiment is designed, three different fluorescence detection principles are used for the determination of caffeine, saccharin and sodium benzoate in beverages. A laser-based indirect fluorometric detection technique in TLC is developed in Section 5. Section 6 is totally different from Sections 1 through 5. An ultrasonic effect on the separation of DNA fragments in agarose gel electrophoresis is investigated. 262 refs.« less

Development and evaluation of a hydrophilic interaction liquid chromatography-MS/MS method to quantify 19 nucleobases and nucleosides in rat plasma.

PubMed

Du, Yan; Li, Yin-Jie; Hu, Xun-Xiu; Deng, Xu; Qian, Zeng-Ting; Li, Zheng; Guo, Meng-Zhe; Tang, Dao-Quan

2017-04-01

As essential endogenous compounds, nucleobases and nucleosides fulfill various functions in living organisms. This study presents the development and validation of a new hydrophilic interaction liquid chromatography tandem mass spectrometry method for simultaneous quantification of 19 nucleobases and nucleosides in rat plasma. For the sample preparation, 15 kinds of protein precipitants were evaluated according to the chromatographic profile and ion response of analytes. The optimization of chromatographic separation was respectively performed using reversed-phase liquid chromatography and hydrophilic interaction liquid chromatography mode; each separation mode included two test columns with different stationary phases. The chromatographic profile and parameters such as half-width (W 1/2 ), capacity factor (K') and tailing factor (f t ) were used to evaluate the separation efficiencies. Furthermore, the adopted composition of two mobile phase systems and the concentrations of the additives in the optimum buffer system were also investigated. The developed method was fully validated and successfully applied quantitatively to determine 19 nucleobases and nucleosides in plasma from normal and diabetic nephropathy (DN) rats. Significant differences between normal and DN rats were found in plasma levels of cytosine, xanthine, thymidine, adenosine, guanosine, inosine and 8-hydroxy-2'-deoxyguanosine. This information may provide a useful reference for the discovery of potential biomarkers of DN. Copyright © 2016 John Wiley & Sons, Ltd.

Method development of enantiomer separations by affinity capillary electrophoresis, cyclodextrin electrokinetic chromatography and capillary electrophoresis-mass spectrometry.

PubMed

Tanaka, Yoshihide

2002-07-01

Capillary electrophoresis (CE) has become a powerful tool for enantiomer separations during the last decade. Since 1993, the author has investigated enantiomer separations by affinity capillary electrophoresis (affinity CE) with some proteins and by cyclodextrin electrokinetic chromatography (CDEKC) with some charged cyclodextrins (CDs). Many successful enantiomer separations are demonstrated from our study in this review article. In the enantiomer separations by affinity CE, the deterioration of detection sensitivity was observed under high concentration of the protein in running solutions. The partial filling technique was practically useful to solve the serious problem. It allowed operation at high protein concentrations, such as 500 mumol/L, without the detection problem. Charged CDs had several advantages for the enantiomer separations over neutral ones. Strong electrostatic interactions between a charged CD and oppositely charged analytes should be effective for the formation of the complex. A large difference in electrophoretic mobility between the free analyte and the inclusion complex should also enhance the enantiomeric resolution. In CE-mass spectrometry (CE-MS), the partial filling technique was applied to avoid the introduction of nonvolatile chiral selectors into the CE-MS interface. By replacing the nonvolatile electrolytes in the running buffer by volatile ones, the separation conditions employed in CE with the UV detection method could be transferred to CE-MS.

Simultaneous determination of phenylethanoid glycosides and aglycones by capillary zone electrophoresis with running buffer modifier.

PubMed

Dong, Shuqing; Gao, Ruibin; Yang, Yan; Guo, Mei; Ni, Jingman; Zhao, Liang

2014-03-15

Although the separation efficiency of capillary electrophoresis (CE) is much higher than that of other chromatographic methods, it is sometimes difficult to adequately separate the complex ingredients in biological samples. This article describes how one effective and simple way to develop the separation efficiency in CE is to add some modifiers to the running buffer. The suitable running buffer modifier β-cyclodextrin (β-CD) was explored to fast and completely separate four phenylethanoid glycosides and aglycones (homovanillyl alcohol, hydroxytyrosol, 3,4-dimethoxycinnamic acid, and caffeic acid) in Lamiophlomis rotata (Lr) and Cistanche by capillary zone electrophoresis with ultraviolet (UV) detection. It was found that when β-CD was used as running buffer modifier, a baseline separation of the four analytes could be accomplished in less than 20 min and the detection limits were as low as 10(-3) mg L(-1). Other factors affecting the CE separation, such as working potential, pH value and ionic strength of running buffer, separation voltage, and sample injection time, were investigated extensively. Under the optimal conditions, a successful practical application on the determination of Lr and Cistanche samples confirmed the validity and practicability of this method. Copyright © 2014 Elsevier Inc. All rights reserved.

Development of an aerodyanmic theory capable of predicting surface loads on slender wings with vortex flow

NASA Technical Reports Server (NTRS)

Gloss, B. B.; Johnson, F. T.

1976-01-01

The Boeing Commercial Airplane Company developed an inviscid three-dimensional lifting surface method that shows promise in being able to accurately predict loads, subsonic and supersonic, on wings with leading-edge separation and reattachment.

Development and optimisation of an HPLC-DAD-ESI-Q-ToF method for the determination of phenolic acids and derivatives.

PubMed

Restivo, Annalaura; Degano, Ilaria; Ribechini, Erika; Colombini, Maria Perla

2014-01-01

A method for the HPLC-MS/MS analysis of phenols, including phenolic acids and naphtoquinones, using an amide-embedded phase column was developed and compared to the literature methods based on classical C18 stationary phase columns. RP-Amide is a recently developed polar embedded stationary phase, whose wetting properties mean that up to 100% water can be used as an eluent. The increased retention and selectivity for polar compounds and the possibility of working in 100% water conditions make this column particularly interesting for the HPLC analysis of phenolic acids and derivatives. In this study, the chromatographic separation was optimised on an HPLC-DAD, and was used to separate 13 standard phenolic acids and derivatives. The method was validated on an HPLC-ESI-Q-ToF. The acquisition was performed in negative polarity and MS/MS target mode. Ionisation conditions and acquisition parameters for the Q-ToF detector were investigated by working on collision energies and fragmentor potentials. The performance of the method was fully evaluated on standards. Moreover, several raw materials containing phenols were analysed: walnut, gall, wine, malbec grape, French oak, red henna and propolis. Our method allowed us to characterize the phenolic composition in a wide range of matrices and to highlight possible matrix effects.

Fast separation and determination of tyrosol, hydroxytyrosol and other phenolic compounds in extra-virgin olive oil by capillary zone electrophoresis with ultraviolet-diode array detection.

PubMed

Bonoli, Matteo; Montanucci, Marina; Gallina Toschi, Tullia; Lercker, Giovanni

2003-09-05

Olive oil is the main source of fat in the Mediterranean diet, and its consumption has been related to a low incidence of coronary heart disease and certain cancers. Recent findings demonstrate that olive oil phenolics are powerful in vitro and in vivo antioxidants and display other biological activities that could partially account for the observed healthful effects of the Mediterranean diet. A detailed method optimization plan was carried out to separate the most popular phenols in olive oil for four separation parameters: buffer concentration, buffer pH, applied voltage and temperature. Consequently, an analytical method capable of separating 21 different phenols and polyphenols by capillary zone electrophoresis was developed; the separation was performed within 10 min, using a 40 cm x 50 microm capillary, with a 45 mM sodium tetraborate buffer (pH 9.60), at 27 kV and 30 degrees C. The optimized method was applied to methanolic extracts of several Italian extra-virgin olive oils obtained by different technologies in order to characterize and to compare their antioxidant profile. Positive correlations of phenolic compounds found by capillary zone electrophoresis (CZE) and two colorimetric indexes (total polyphenols and o-diphenols) were found and discussed.

A four dimensional separation method based on continuous heart-cutting gas chromatography with ion mobility and high resolution mass spectrometry.

PubMed

Lipok, Christian; Hippler, Jörg; Schmitz, Oliver J

2018-02-09

A two-dimensional GC (2D-GC) method was developed and coupled to an ion mobility-high resolution mass spectrometer, which enables the separation of complex samples in four dimensions (2D-GC, ion mobilility spectrometry and mass spectrometry). This approach works as a continuous multiheart-cutting GC-system (GC+GC), using a long modulation time of 20s, which allows the complete transfer of most of the first dimension peaks to the second dimension column without fractionation, in comparison to comprehensive two-dimensional gas chromatography (GCxGC). Hence, each compound delivers only one peak in the second dimension, which simplifies the data handling even when ion mobility spectrometry as a third and mass spectrometry as a fourth dimension are introduced. The analysis of a plant extract from Calendula officinales shows the separation power of this four dimensional separation method. The introduction of ion mobility spectrometry provides an additional separation dimension and allows to determine collision cross sections (CCS) of the analytes as a further physicochemical constant supporting the identification. A CCS database with more than 800 standard substances including drug-like compounds and pesticides was used for CCS data base search in this work. Copyright © 2017 Elsevier B.V. All rights reserved.

Evaluation of tannins interactions in grape (Vitis vinifera L.) skins.

PubMed

Rustioni, Laura; Fiori, Simone; Failla, Osvaldo

2014-09-15

Tannins have a central role in grapevine berries both for their physiological and enological implications. In the skin tissue they can be in vacuolar solution, or associated to the cell walls through weak or strong physicochemical interactions. The present work aims to separate vacuolar, non-covalently and covalently bonded tannins fractions. A specific extraction procedure was developed. A first extraction in ethanol at low temperature allowed the quantification of vacuolar tannins. An urea treatment followed by an ethanol extraction at room temperature was able to separate non-covalently bonded compounds. Finally an acid catalysis was used to break down proanthocyanidin covalent bonds. The method was validated on ripe grape samples of three cultivars, on berries developed in two sun exposure conditions. The Ethephon treatment effect was also evaluated. Beside the method development, a preliminary evaluation of the cultivar, exposition and Ethephon treatment effects are discussed. Copyright © 2014 Elsevier Ltd. All rights reserved.

Rapid quantification of underivatized amino acids in plasma by hydrophilic interaction liquid chromatography (HILIC) coupled with tandem mass-spectrometry.

PubMed

Prinsen, Hubertus C M T; Schiebergen-Bronkhorst, B G M; Roeleveld, M W; Jans, J J M; de Sain-van der Velden, M G M; Visser, G; van Hasselt, P M; Verhoeven-Duif, N M

2016-09-01

Amino acidopathies are a class of inborn errors of metabolism (IEM) that can be diagnosed by analysis of amino acids (AA) in plasma. Current strategies for AA analysis include cation exchange HPLC with post-column ninhydrin derivatization, GC-MS, and LC-MS/MS-related methods. Major drawbacks of the current methods are time-consuming procedures, derivative problems, problems with retention, and MS-sensitivity. The use of hydrophilic interaction liquid chromatography (HILIC) columns is an ideal separation mode for hydrophilic compounds like AA. Here we report a HILIC-method for analysis of 36 underivatized AA in plasma to detect defects in AA metabolism that overcomes the major drawbacks of other methods. A rapid, sensitive, and specific method was developed for the analysis of AA in plasma without derivatization using HILIC coupled with tandem mass-spectrometry (Xevo TQ, Waters). Excellent separation of 36 AA (24 quantitative/12 qualitative) in plasma was achieved on an Acquity BEH Amide column (2.1×100 mm, 1.7 μm) in a single MS run of 18 min. Plasma of patients with a known IEM in AA metabolism was analyzed and all patients were correctly identified. The reported method analyzes 36 AA in plasma within 18 min and provides baseline separation of isomeric AA such as leucine and isoleucine. No separation was obtained for isoleucine and allo-isoleucine. The method is applicable to study defects in AA metabolism in plasma.

Optimizing and developing a continuous separation system for the wet process separation of aluminum and polyethylene in aseptic composite packaging waste.

PubMed

Yan, Dahai; Peng, Zheng; Liu, Yuqiang; Li, Li; Huang, Qifei; Xie, Minghui; Wang, Qi

2015-01-01

The consumption of milk in China is increasing as living standards rapidly improve, and huge amounts of aseptic composite milk packaging waste are being generated. Aseptic composite packaging is composed of paper, polyethylene, and aluminum. It is difficult to separate the polyethylene and aluminum, so most of the waste is currently sent to landfill or incinerated with other municipal solid waste, meaning that enormous amounts of resources are wasted. A wet process technique for separating the aluminum and polyethylene from the composite materials after the paper had been removed from the original packaging waste was studied. The separation efficiency achieved using different separation reagents was compared, different separation mechanisms were explored, and the impacts of a range of parameters, such as the reagent concentration, temperature, and liquid-solid ratio, on the separation time and aluminum loss ratio were studied. Methanoic acid was found to be the optimal separation reagent, and the suitable conditions were a reagent concentration of 2-4 mol/L, a temperature of 60-80°C, and a liquid-solid ratio of 30 L/kg. These conditions allowed aluminum and polyethylene to be separated in less than 30 min, with an aluminum loss ratio of less than 3%. A mass balance was produced for the aluminum-polyethylene separation system, and control technique was developed to keep the ion concentrations in the reaction system stable. This allowed a continuous industrial-scale process for separating aluminum and polyethylene to be developed, and a demonstration facility with a capacity of 50t/d was built. The demonstration facility gave polyethylene and aluminum recovery rates of more than 98% and more than 72%, respectively. Separating 1t of aluminum-polyethylene composite packaging material gave a profit of 1769 Yuan, meaning that an effective method for recycling aseptic composite packaging waste was achieved. Copyright © 2014 Elsevier Ltd. All rights reserved.

Bioprocessing development: Immune/cellular applications: Anti-Ig autoantibody and complement-mediated destruction of neoplastic cells

NASA Technical Reports Server (NTRS)

Twomey, J. J.

1976-01-01

This space bioprocessing contract effort was comprised of four general objectives. These were: (1) the evaluation of current separation processes, (2) the identification of problems relevant to the separation of important biologicals, (3) the identification of ground-based assay methods needed for pre- and postflight analysis of space bioprocessing separation technology; and (4) the establishment of methods to determine the efficiency of space bioprocessing separation procedures. Immunology was deemed advantageous to study the diversity of cells and cell products involved and the extensive interest being given to their separation. Upon recognition of a cellular or molecular agent as foreign to the body, the immune system becomes activated to produce cells whose function is to destroy that agent and cell products whose function is to inactivate the agent and assist in its destruction. Long after the agent is removed from the body, some cells remain in a state of readiness to continue these destructive actions specifically against that agent should further exposure to it occur. This is the basis of acquired immunity to disease.

Contributions of immunoaffinity chromatography to deep proteome profiling of human biofluids

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wu, Chaochao; Duan, Jicheng; Liu, Tao

2016-05-01

Human biofluids, especially blood plasma or serum, hold great potential as the sources of potential biomarkers for various diseases; however, the enormous dynamic range of protein concentrations in biofluids represents a significant analytical challenge to detect promising low-abundance protein biomarkers. Over the last decade, various immunoaffinity chromatographic methods have been developed and routinely applied for separating low-abundance proteins from the high and moderate-abundance proteins, thus enabling more effective detection of low-abundance proteins. Herein, we review the advances of immunoaffinity separation methods and their contributions to the proteomics applications of different human biofluids. The limitations and future perspective of immunoaffinity separationmore » methods are also discussed.« less

A vortex-filament and core model for wings with edge vortex separation

NASA Technical Reports Server (NTRS)

Pao, J. L.; Lan, C. E.

1981-01-01

A method for predicting aerodynamic characteristics of slender wings with edge vortex separation was developed. Semiempirical but simple methods were used to determine the initial positions of the free sheet and vortex core. Comparison with available data indicates that: the present method is generally accurate in predicting the lift and induced drag coefficients but the predicted pitching moment is too positive; the spanwise lifting pressure distributions estimated by the one vortex core solution of the present method are significantly better than the results of Mehrotra's method relative to the pressure peak values for the flat delta; the two vortex core system applied to the double delta and strake wing produce overall aerodynamic characteristics which have good agreement with data except for the pitching moment; and the computer time for the present method is about two thirds of that of Mehrotra's method.

A vortex-filament and core model for wings with edge vortex separation

NASA Technical Reports Server (NTRS)

Pao, J. L.; Lan, C. E.

1982-01-01

A vortex filament-vortex core method for predicting aerodynamic characteristics of slender wings with edge vortex separation was developed. Semi-empirical but simple methods were used to determine the initial positions of the free sheet and vortex core. Comparison with available data indicates that: (1) the present method is generally accurate in predicting the lift and induced drag coefficients but the predicted pitching moment is too positive; (2) the spanwise lifting pressure distributions estimated by the one vortex core solution of the present method are significantly better than the results of Mehrotra's method relative to the pressure peak values for the flat delta; (3) the two vortex core system applied to the double delta and strake wings produce overall aerodynamic characteristics which have good agreement with data except for the pitching moment; and (4) the computer time for the present method is about two thirds of that of Mehrotra's method.

Optic disk localization by a robust fusion method

NASA Astrophysics Data System (ADS)

Zhang, Jielin; Yin, Fengshou; Wong, Damon W. K.; Liu, Jiang; Baskaran, Mani; Cheng, Ching-Yu; Wong, Tien Yin

2013-02-01

The optic disk localization plays an important role in developing computer-aided diagnosis (CAD) systems for ocular diseases such as glaucoma, diabetic retinopathy and age-related macula degeneration. In this paper, we propose an intelligent fusion of methods for the localization of the optic disk in retinal fundus images. Three different approaches are developed to detect the location of the optic disk separately. The first method is the maximum vessel crossing method, which finds the region with the most number of blood vessel crossing points. The second one is the multichannel thresholding method, targeting the area with the highest intensity. The final method searches the vertical and horizontal region-of-interest separately on the basis of blood vessel structure and neighborhood entropy profile. Finally, these three methods are combined using an intelligent fusion method to improve the overall accuracy. The proposed algorithm was tested on the STARE database and the ORIGAlight database, each consisting of images with various pathologies. The preliminary result on the STARE database can achieve 81.5%, while a higher result of 99% can be obtained for the ORIGAlight database. The proposed method outperforms each individual approach and state-of-the-art method which utilizes an intensity-based approach. The result demonstrates a high potential for this method to be used in retinal CAD systems.

Imaging cell picker: A morphology-based automated cell separation system on a photodegradable hydrogel culture platform.

PubMed

Shibuta, Mayu; Tamura, Masato; Kanie, Kei; Yanagisawa, Masumi; Matsui, Hirofumi; Satoh, Taku; Takagi, Toshiyuki; Kanamori, Toshiyuki; Sugiura, Shinji; Kato, Ryuji

2018-06-09

Cellular morphology on and in a scaffold composed of extracellular matrix generally represents the cellular phenotype. Therefore, morphology-based cell separation should be interesting method that is applicable to cell separation without staining surface markers in contrast to conventional cell separation methods (e.g., fluorescence activated cell sorting and magnetic activated cell sorting). In our previous study, we have proposed a cloning technology using a photodegradable gelatin hydrogel to separate the individual cells on and in hydrogels. To further expand the applicability of this photodegradable hydrogel culture platform, we here report an image-based cell separation system imaging cell picker for the morphology-based cell separation on a photodegradable hydrogel. We have developed the platform which enables the automated workflow of image acquisition, image processing and morphology analysis, and collection of a target cells. We have shown the performance of the morphology-based cell separation through the optimization of the critical parameters that determine the system's performance, such as (i) culture conditions, (ii) imaging conditions, and (iii) the image analysis scheme, to actually clone the cells of interest. Furthermore, we demonstrated the morphology-based cloning performance of cancer cells in the mixture of cells by automated hydrogel degradation by light irradiation and pipetting. Copyright © 2018 The Society for Biotechnology, Japan. Published by Elsevier B.V. All rights reserved.

ANALYSIS OF SELECTED PYRETHROID PESTICIDES USING REVERSE PHASE HIGH PRESSURE LIQUID CHROMATOGRAPHY/UV

EPA Science Inventory

This research was conducted in cooperation with EPA Region 4 in Athens, GA to develop a method to analyze selected pyrethroid pesticides using Reverse Phase-High Pressure Liquid Chromatography (HPLC). This HPLC method will aid researchers in separating and identifying these py...

Diffraction as a Method of Critical Policy Analysis

ERIC Educational Resources Information Center

Ulmer, Jasmine B.

2016-01-01

Recent developments in critical policy analysis have occurred alongside the new materialisms in qualitative research. These lines of scholarship have unfolded along two separate, but related, tracks. In particular, the new materialist method of "diffraction" aligns with many elements of critical policy analysis. Both involve critical…

Chemical speciation and recovery of gold(I, III) from wastewater and silver by liquid-liquid extraction with the ion-pair reagent amiloride mono hydrochloride and AAS determination.

PubMed

El-Shahawi, M S; Bashammakh, A S; Bahaffi, S O

2007-06-15

A novel and low cost liquid-liquid extraction procedure for the separation of gold(III) at trace level from aqueous medium of pH 5-9 has been developed. The method has been based upon the formation of a yellow colored ternary complex ion associate of tetrachloro gold(III) complex anion, AuCl(4)(-) with the ion-pair reagent 1-(3,5-diamino-6-chloropyrazinecarboxyl) guanidine hydrochloride monohydrate, namely amiloride, DPG(+).Cl(-). The effect of various parameters, e.g. pH, organic solvent, shaking time, etc. on the preconcentration of gold(III) from the aqueous media by the DPG(+).Cl(-) reagent has been investigated. The colored gold species was quantitatively extracted into 4-methyl pentan-2-one. The chemical composition of the ion associate of DPG(+).Cl(-) with AuCl(4)(-) in the organic solvent has been determined by the Job's method. The molar absorptivity (2.19x10(4)Lmol(-1)cm(-1)) of the associate DPG(+).AuCl(4)(-) at 362nm enabled a convenient application of the developed extraction procedure for the separation and AAS determination of traces of aurate ions. Mono-valence gold ions after oxidation to gold(III) with bromine water in HCl (1.0molL(-1)) media have been also extracted quantitatively from the aqueous media by the developed procedure. The chemical speciation of mono- and/or tri-valence gold species spiked to fresh and industrial wastewater samples has been achieved. The method has been also applied successfully from the separation of gold(I) and gold(III) species from metallic ions and silver. The developed method has also the advantage of freedom from most diverse ions.

Intelligent peak deconvolution through in-depth study of the data matrix from liquid chromatography coupled with a photo-diode array detector applied to pharmaceutical analysis.

PubMed

Arase, Shuntaro; Horie, Kanta; Kato, Takashi; Noda, Akira; Mito, Yasuhiro; Takahashi, Masatoshi; Yanagisawa, Toshinobu

2016-10-21

Multivariate curve resolution-alternating least squares (MCR-ALS) method was investigated for its potential to accelerate pharmaceutical research and development. The fast and efficient separation of complex mixtures consisting of multiple components, including impurities as well as major drug substances, remains a challenging application for liquid chromatography in the field of pharmaceutical analysis. In this paper we suggest an integrated analysis algorithm functioning on a matrix of data generated from HPLC coupled with photo-diode array detector (HPLC-PDA) and consisting of the mathematical program for the developed multivariate curve resolution method using an expectation maximization (EM) algorithm with a bidirectional exponentially modified Gaussian (BEMG) model function as a constraint for chromatograms and numerous PDA spectra aligned with time axis. The algorithm provided less than ±1.0% error between true and separated peak area values at resolution (R s ) of 0.6 using simulation data for a three-component mixture with an elution order of a/b/c with similarity (a/b)=0.8410, (b/c)=0.9123 and (a/c)=0.9809 of spectra at peak apex. This software concept provides fast and robust separation analysis even when method development efforts fail to achieve complete separation of the target peaks. Additionally, this approach is potentially applicable to peak deconvolution, allowing quantitative analysis of co-eluted compounds having exactly the same molecular weight. This is complementary to the use of LC-MS to perform quantitative analysis on co-eluted compounds using selected ions to differentiate the proportion of response attributable to each compound. Copyright © 2016 Elsevier B.V. All rights reserved.

Artificial Satellites Observations Using the Complex of Telescopes of RI "MAO"

NASA Astrophysics Data System (ADS)

Sybiryakova, Ye. S.; Shulga, O. V.; Vovk, V. S.; Kaliuzny, M. P.; Bushuev, F. I.; Kulichenko, M. O.; Haloley, M. I.; Chernozub, V. M.

2017-02-01

Special methods, means and software for cosmic objects' observation and processing of obtained results were developed. Combined method, which consists in separated accumulation of images of reference stars and artificial objects, is the main method used in observations of artificial cosmic objects. It is used for observations of artificial objects at all types of orbits.

Energy conversion and storage program

NASA Astrophysics Data System (ADS)

Cairns, E. J.

1992-03-01

The Energy Conversion and Storage Program applies chemistry and materials science principles to solve problems in: (1) production of new synthetic fuels; (2) development of high-performance rechargeable batteries and fuel cells; (3) development of advanced thermochemical processes for energy conversion; (4) characterization of complex chemical processes; and (5) application of novel materials for energy conversion and transmission. Projects focus on transport-process principles, chemical kinetics, thermodynamics, separation processes, organic and physical chemistry, novel materials, and advanced methods of analysis. Electrochemistry research aims to develop advanced power systems for electric vehicle and stationary energy storage applications. Topics include identification of new electrochemical couples for advanced rechargeable batteries, improvements in battery and fuel-cell materials, and the establishment of engineering principles applicable to electrochemical energy storage and conversion. Chemical Applications research includes topics such as separations, catalysis, fuels, and chemical analyses. Included in this program area are projects to develop improved, energy-efficient methods for processing waste streams from synfuel plants and coal gasifiers. Other research projects seek to identify and characterize the constituents of liquid fuel-system streams and to devise energy-efficient means for their separation. Materials Applications research includes the evaluation of the properties of advanced materials, as well as the development of novel preparation techniques. For example, the use of advanced techniques, such as sputtering and laser ablation, are being used to produce high-temperature superconducting films.

Two inviscid computational simulations of separated flow about airfoils

NASA Technical Reports Server (NTRS)

Barnwell, R. W.

1976-01-01

Two inviscid computational simulations of separated flow about airfoils are described. The basic computational method is the line relaxation finite-difference method. Viscous separation is approximated with inviscid free-streamline separation. The point of separation is specified, and the pressure in the separation region is calculated. In the first simulation, the empiricism of constant pressure in the separation region is employed. This empiricism is easier to implement with the present method than with singularity methods. In the second simulation, acoustic theory is used to determine the pressure in the separation region. The results of both simulations are compared with experiment.

Disaggregating tree and grass phenology in tropical savannas

NASA Astrophysics Data System (ADS)

Zhou, Qiang

Savannas are mixed tree-grass systems and as one of the world's largest biomes represent an important component of the Earth system affecting water and energy balances, carbon sequestration and biodiversity as well as supporting large human populations. Savanna vegetation structure and its distribution, however, may change because of major anthropogenic disturbances from climate change, wildfire, agriculture, and livestock production. The overstory and understory may have different water use strategies, different nutrient requirements and have different responses to fire and climate variation. The accurate measurement of the spatial distribution and structure of the overstory and understory are essential for understanding the savanna ecosystem. This project developed a workflow for separating the dynamics of the overstory and understory fractional cover in savannas at the continental scale (Australia, South America, and Africa). Previous studies have successfully separated the phenology of Australian savanna vegetation into persistent and seasonal greenness using time series decomposition, and into fractions of photosynthetic vegetation (PV), non-photosynthetic vegetation (NPV) and bare soil (BS) using linear unmixing. This study combined these methods to separate the understory and overstory signal in both the green and senescent phenological stages using remotely sensed imagery from the MODIS (MODerate resolution Imaging Spectroradiometer) sensor. The methods and parameters were adjusted based on the vegetation variation. The workflow was first tested at the Australian site. Here the PV estimates for overstory and understory showed best performance, however NPV estimates exhibited spatial variation in validation relationships. At the South American site (Cerrado), an additional method based on frequency unmixing was developed to separate green vegetation components with similar phenology. When the decomposition and frequency methods were compared, the frequency method was better for extracting the green tree phenology, but the original decomposition method was better for retrieval of understory grass phenology. Both methods, however, were less accurate than in the Cerrado than in Australia due to intermingling and intergrading of grass and small woody components. Since African savanna trees are predominantly deciduous, the frequency method was combined with the linear unmixing of fractional cover to attempt to separate the relatively similar phenology of deciduous trees and seasonal grasses. The results for Africa revealed limitations associated with both methods. There was spatial and seasonal variation in the spectral indices used to unmix fractional cover resulting in poor validation for NPV in particular. The frequency analysis revealed significant phase variation indicative of different phenology, but these could not be clearly ascribed to separate grass and tree components. Overall findings indicate that site-specific variation and vegetation structure and composition, along with MODIS pixel resolution, and the simple vegetation index approach used was not robust across the different savanna biomes. The approach showed generally better performance for estimating PV fraction, and separating green phenology, but there were major inconsistencies, errors and biases in estimation of NPV and BS outside of the Australian savanna environment.

Fast analysis of capsaicinoids in Naga Jolokia extracts (Capsicum chinense) by high-performance liquid chromatography using fused core columns.

PubMed

Stipcovich, Tea; Barbero, Gerardo F; Ferreiro-González, Marta; Palma, Miguel; Barroso, Carmelo G

2018-01-15

A rapid high-performance liquid chromatography method with a C18 reverse-phase fused-core column has been developed for the determination and quantification of the main capsaicinoids (nornordihydrocapsaicin, nordihydrocapsaicin, capsaicin, dihydrocapsaicin, homocapsaicin and homodihydrocapsaicin) present in Naga Jolokia peppers. A fused-core Kinetex™ C18 column (50×2.1mm i.d.; 2.6μm) was used for the analysis. The chromatographic separation was obtained with a gradient method in which the mobile phase was water (0.1% acetic acid) as solvent A and acetonitrile (0.1% acetic acid) as solvent B. The separation of all compounds was achieved in less than 3min with a total analysis time (sample-to-sample) of 10min. The robustness of the method was evaluated. The method showed excellent repeatability and intermediate precision expressed as coefficient of variance of less than 2%. The developed method was employed for the quantification of the major capsaicinoids present in different peppers and commercial products containing chilli peppers. Copyright © 2017 Elsevier Ltd. All rights reserved.

Recent developments in separation of low molecular weight heparin anticoagulants.

PubMed

Sadowski, Radosław; Gadzała-Kopciuch, Renata; Buszewski, Bogusław

2017-10-05

The general function of anticoagulants is to prevent blood clotting and growing of the existing clots in blood vessels. In recent years, there has been a significant improvement in developing methods of prevention as well as pharmacologic and surgical treatment of thrombosis. For over the last two decades, low molecular weight heparins (LMWHs) have found their application in the antithrombotic diseases treatment. These types of drugs are widely used in clinical therapy. Despite the biological and medical importance of LMWHs, they have not been completely characterized in terms of their chemical structure. Due to both, the structural complexity of these anticoagulants and the presence of impurities, their structural characterization requires the employment of advanced analytical techniques. Since separation techniques play the key role in these endeavors, this review will focus on the presentation of recent developments in the separation of LMWH anticoagulants. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

Electrophoresis for the analysis of heparin purity and quality.

PubMed

Volpi, Nicola; Maccari, Francesca; Suwan, Jiraporn; Linhardt, Robert J

2012-06-01

The adulteration of raw heparin with oversulfated chondroitin sulfate (OSCS) in 2007-2008 produced a global crisis resulting in extensive revisions to the pharmacopeia monographs and prompting the FDA to recommend the development of additional methods for the analysis of heparin purity. As a consequence, a wide variety of innovative analytical approaches have been developed for the quality assurance and purity of unfractionated and low-molecular-weight heparins. This review discusses recent developments in electrophoresis techniques available for the sensitive separation, detection, and partial structural characterization of heparin contaminants. In particular, this review summarizes recent publications on heparin quality and related impurity analysis using electrophoretic separations such as capillary electrophoresis (CE) of intact polysaccharides and hexosamines derived from their acidic hydrolysis, and polyacrylamide gel electrophoresis (PAGE) for the separation of heparin samples without and in the presence of its relatively specific depolymerization process with nitrous acid treatment. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Quantification of false positive reduction in nucleic acid purification on hemorrhagic fever DNA.

DOE Office of Scientific and Technical Information (OSTI.GOV)

James, Conrad D.; Pohl, Kenneth Roy; Derzon, Mark Steven

2006-11-01

Columbia University has developed a sensitive highly multiplexed system for genetic identification of nucleic acid targets. The primary obstacle to implementing this technology is the high rate of false positives due to high levels of unbound reporters that remain within the system after hybridization. The ability to distinguish between free reporters and reporters bound to targets limits the use of this technology. We previously demonstrated a new electrokinetic method for binary separation of kb pair long DNA molecules and oligonucleotides. The purpose of this project 99864 is to take these previous demonstrations and further develop the technique and hardware formore » field use. Specifically, our objective was to implement separation in a heterogeneous sample (containing target DNA and background oligo), to perform the separation in a flow-based device, and to develop all of the components necessary for field testing a breadboard prototype system.« less

Electrophoresis for the analysis of heparin purity and quality

PubMed Central

Volpi, Nicola; Maccari, Francesca; Suwan, Jiraporn; Linhardt, Robert J.

2012-01-01

The adulteration of raw heparin with oversulfated chondroitin sulfate (OSCS) in 2007–2008 produced a global crisis resulting in extensive revisions to the pharmacopeia monographs and prompting the FDA to recommend the development of additional methods for the analysis of heparin purity. As a consequence, a wide variety of innovative analytical approaches have been developed for the quality assurance and purity of unfractionated and low-molecular-weight heparins. This review discusses recent developments in electrophoresis techniques available for the sensitive separation, detection, and partial structural characterization of heparin contaminants. In particular, this review summarizes recent publications on heparin quality and related impurity analysis using electrophoretic separations such as capillary electrophoresis (CE) of intact polysaccharides and hexosamines derived from their acidic hydrolysis, and polyacrylamide gel electrophoresis (PAGE) for the separation of heparin samples without and in the presence of its relatively specific depolymerization process with nitrous acid treatment. PMID:22736353

Nonlinear multi-photon laser wave-mixing optical detection in microarrays and microchips for ultrasensitive detection and separation of biomarkers for cancer and neurodegenerative diseases

NASA Astrophysics Data System (ADS)

Iwabuchi, Manna; Hetu, Marcel; Maxwell, Eric; Pradel, Jean S.; Ramos, Sashary; Tong, William G.

2015-09-01

Multi-photon degenerate four-wave mixing is demonstrated as an ultrasensitive absorption-based optical method for detection, separation and identification of biomarker proteins in the development of early diagnostic methods for HIV- 1, cancer and neurodegenerative diseases using compact, portable microarrays and capillary- or microchip-based chemical separation systems that offer high chemical specificity levels. The wave-mixing signal has a quadratic dependence on concentration, and hence, it allows more reliable monitoring of smaller changes in analyte properties. Our wave-mixing detection sensitivity is comparable or better than those of current methods including enzyme-linked immunoassay for clinical diagnostic and screening. Detection sensitivity is excellent since the wave-mixing signal is a coherent laser-like beam that can be collected with virtually 100% collection efficiency with high S/N. Our analysis time is short (1-15 minutes) for molecular weight-based protein separation as compared to that of a conventional separation technique, e.g., sodium dodecyl sulfate-polyacrylamide gel electrophoresis. When ultrasensitive wavemixing detection is paired with high-resolution capillary- or microchip-based separation systems, biomarkers can be separated and identified at the zepto- and yocto-mole levels for a wide range of analytes. Specific analytes can be captured in a microchannel through the use of antibody-antigen interactions that provide better chemical specificity as compared to size-based separation alone. The technique can also be combined with immune-precipitation and a multichannel capillary array for high-throughput analysis of more complex protein samples. Wave mixing allows the use of chromophores and absorption-modifying tags, in addition to conventional fluorophores, for online detection of immunecomplexes related to cancer.

Evaluation of Mars CO2 Capture and Gas Separation Technologies

NASA Technical Reports Server (NTRS)

Muscatello, Anthony C.; Santiago-Maldonado, Edgardo; Gibson, Tracy; Devor, Robert; Captain, James

2011-01-01

Recent national policy statements have established that the ultimate destination of NASA's human exploration program is Mars. In Situ Resource Utilization (ISRU) is a key technology required to ,enable such missions and it is appropriate to review progress in this area and continue to advance the systems required to produce rocket propellant, oxygen, and other consumables on Mars using the carbon dioxide atmosphere and other potential resources. The Mars Atmospheric Capture and Gas separation project is selecting, developing, and demonstrating techniques to capture and purify Martian atmospheric gases for their utilization for the production of hydrocarbons, oxygen, and water in ISRU systems. Trace gases will be required to be separated from Martian atmospheric gases to provide pure CO2 to processing elements. In addition, other Martian gases, such as nitrogen and argon, occur in concentrations high enough to be useful as buffer gas and should be captured as well. To achieve these goals, highly efficient gas separation processes will be required. These gas separation techniques are also required across various areas within the ISRU project to support various consumable production processes. The development of innovative gas separation techniques will evaluate the current state-of-the-art for the gas separation required, with the objective to demonstrate and develop light-weight, low-power methods for gas separation. Gas separation requirements include, but are not limited to the selective separation of: (1) methane and water from unreacted carbon oxides (C02-CO) and hydrogen typical of a Sabatier-type process, (2) carbon oxides and water from unreacted hydrogen from a Reverse Water-Gas Shift process, (3)/carbon oxides from oxygen from a trash/waste processing reaction, and (4) helium from hydrogen or oxygen from a propellant scavenging process. Potential technologies for the separations include' freezers, selective membranes, selective solvents, polymeric sorbents, zeolites, and new technologies. This paper summarizes the results of an extensive literature review of candidate technologies for the capture and separation of CO2 and other relevant gases. This information will be used to prioritize the technologies to be developed further during this and other ISRU projects.

Hydrodynamic injection with pneumatic valving for microchip electrophoresis with total analyte utilization

PubMed Central

Sun, Xuefei; Kelly, Ryan T.; Danielson, William F.; Agrawal, Nitin; Tang, Keqi; Smith, Richard D.

2011-01-01

A novel hydrodynamic injector that is directly controlled by a pneumatic valve has been developed for reproducible microchip capillary electrophoresis (CE) separations. The poly(dimethylsiloxane) (PDMS) devices used for evaluation comprise a separation channel, a side channel for sample introduction, and a pneumatic valve aligned at the intersection of the channels. A low pressure (≤ 3 psi) applied to the sample reservoir is sufficient to drive sample into the separation channel. The rapidly actuated pneumatic valve enables injection of discrete sample plugs as small as ~100 pL for CE separation. The injection volume can be easily controlled by adjusting the intersection geometry, the solution back pressure and the valve actuation time. Sample injection could be reliably operated at different frequencies (< 0.1 Hz to >2 Hz) with good reproducibility (peak height relative standard deviation ≤ 3.6%) and no sampling biases associated with the conventional electrokinetic injections. The separation channel was dynamically coated with a cationic polymer, and FITC-labeled amino acids were employed to evaluate the CE separation. Highly efficient (≥ 7.0 × 103 theoretical plates for the ~2.4 cm long channel) and reproducible CE separations were obtained. The demonstrated method has numerous advantages compared with the conventional techniques, including repeatable and unbiased injections, little sample waste, high duty cycle, controllable injected sample volume, and fewer electrodes with no need for voltage switching. The prospects of implementing this injection method for coupling multidimensional separations, for multiplexing CE separations and for sample-limited bioanalyses are discussed. PMID:21520147

Development of an on-line flow injection Sr/matrix separation method for accurate, high-throughput determination of Sr isotope ratios by multiple collector-inductively coupled plasma-mass spectrometry.

PubMed

Galler, Patrick; Limbeck, Andreas; Boulyga, Sergei F; Stingeder, Gerhard; Hirata, Takafumi; Prohaska, Thomas

2007-07-01

This work introduces a newly developed on-line flow injection (FI) Sr/Rb separation method as an alternative to the common, manual Sr/matrix batch separation procedure, since total analysis time is often limited by sample preparation despite the fast rate of data acquisition possible by inductively coupled plasma-mass spectrometers (ICPMS). Separation columns containing approximately 100 muL of Sr-specific resin were used for on-line FI Sr/matrix separation with subsequent determination of (87)Sr/(86)Sr isotope ratios by multiple collector ICPMS. The occurrence of memory effects exhibited by the Sr-specific resin, a major restriction to the repetitive use of this costly material, could successfully be overcome. The method was fully validated by means of certified reference materials. A set of two biological and six geological Sr- and Rb-bearing samples was successfully characterized for its (87)Sr/(86)Sr isotope ratios with precisions of 0.01-0.04% 2 RSD (n = 5-10). Based on our measurements we suggest (87)Sr/(86)Sr isotope ratios of 0.713 15 +/- 0.000 16 (2 SD) and 0.709 31 +/- 0.000 06 (2 SD) for the NIST SRM 1400 bone ash and the NIST SRM 1486 bone meal, respectively. Measured (87)Sr/(86)Sr isotope ratios for five basalt samples are in excellent agreement with published data with deviations from the published value ranging from 0 to 0.03%. A mica sample with a Rb/Sr ratio of approximately 1 was successfully characterized for its (87)Sr/(86)Sr isotope signature to be 0.718 24 +/- 0.000 29 (2 SD) by the proposed method. Synthetic samples with Rb/Sr ratios of up to 10/1 could successfully be measured without significant interferences on mass 87, which would otherwise bias the accuracy and uncertainty of the obtained data.

A rapid method for quantification of 242Pu in urine using extraction chromatography and ICP-MS

DOE PAGES

Gallardo, Athena Marie; Than, Chit; Wong, Carolyn; ...

2017-01-01

Occupational exposure to plutonium is generally monitored through analysis of urine samples. Typically, plutonium is separated from the sample and other actinides, and the concentration is determined using alpha spectroscopy. Current methods for separations and analysis are lengthy and require long count times. A new method for monitoring occupational exposure levels of plutonium has been developed, which requires fewer steps and overall less time than the alpha spectroscopy method. In this method, the urine is acidified, and a 239Pu internal standard is added. The urine is digested in a microwave oven, and plutonium is separated using an Eichrom TRU Resinmore » column. The plutonium is eluted, and the eluant is injected directly into the Inductively Coupled Plasma–Mass Spectrometer (ICP-MS). Compared to a direct “dilute and shoot” method, a 30-fold improvement in sensitivity is achieved. This method was validated by analyzing several batches of spiked samples. Based on these analyses, a combined standard uncertainty plot, which relates uncertainty to concentration, was produced. As a result, the MDA 95 was calculated to be 7.0 × 10 –7 μg L –1, and the Lc95 was calculated to be 3.5 × 10 –7 μg L –1 for this method.« less

Sample-independent approach to normalize two-dimensional data for orthogonality evaluation using whole separation space scaling.

PubMed

Jáčová, Jaroslava; Gardlo, Alžběta; Friedecký, David; Adam, Tomáš; Dimandja, Jean-Marie D

2017-08-18

Orthogonality is a key parameter that is used to evaluate the separation power of chromatography-based two-dimensional systems. It is necessary to scale the separation data before the assessment of the orthogonality. Current scaling approaches are sample-dependent, and the extent of the retention space that is converted into a normalized retention space is set according to the retention times of the first and last analytes contained in a unique sample to elute. The presence or absence of a highly retained analyte in a sample can thus significantly influence the amount of information (in terms of the total amount of separation space) contained in the normalized retention space considered for the calculation of the orthogonality. We propose a Whole Separation Space Scaling (WOSEL) approach that accounts for the whole separation space delineated by the analytical method, and not the sample. This approach enables an orthogonality-based evaluation of the efficiency of the analytical system that is independent of the sample selected. The WOSEL method was compared to two currently used orthogonality approaches through the evaluation of in silico-generated chromatograms and real separations of human biofluids and petroleum samples. WOSEL exhibits sample-to-sample stability values of 3.8% on real samples, compared to 7.0% and 10.1% for the two other methods, respectively. Using real analyses, we also demonstrate that some previously developed approaches can provide misleading conclusions on the overall orthogonality of a two-dimensional chromatographic system. Copyright © 2017 Elsevier B.V. All rights reserved.

Separation and quantification of 15 carotenoids by reversed phase high performance liquid chromatography coupled to diode array detection with isosbestic wavelength approach.

PubMed

Mitrowska, Kamila; Vincent, Ursula; von Holst, Christoph

2012-04-13

The manuscript presents the development of a new reverse phase high performance liquid chromatography (RP-HPLC) photo diode array detection method allowing the separation and quantification of 15 carotenoids (adonirubin, adonixanthin, astaxanthin, astaxanthin dimethyl disuccinate, asteroidenone, beta-apo-8'-carotenal, beta-apo-8'-carotenoic acid ethyl ester, beta-carotene, canthaxanthin, capsanthin, citranaxanthin, echinenone, lutein, lycopene, and zeaxanthin), 10 of which are feed additives authorised within the European Union. The developed method allows for the reliable determination of the total carotenoid content in one run using the corresponding E-isomer as calibration standard while taking into account the E/Z-isomers composition. This is a key criterion for the application of the method, since for most of the analytes included in this study analytical standards are only available for the E-isomers. This goal was achieved by applying the isosbestic concept, in order to identify specific wavelengths, at which the absorption coefficients are identical for all stereoisomers concerned. The second target referred to the optimisation of the LC conditions. By means of an experimental design, an optimised RP-HPLC method was developed allowing for a sufficient chromatographic separation of all carotenoids. The selected method uses a Suplex pKb-100 HPLC column and applying a gradient with a mixture of acetonitrile, tert-butyl-methyl ether and water as mobile phases. The limits of detection and limits of quantification ranged from 0.06 mg L(-1) to 0.14 mg L(-1) and from 0.20 mg L(-1) to 0.48 mg L(-1), respectively. Copyright © 2012 Elsevier B.V. All rights reserved.

Stability-Indicating HPTLC Method for Studying Stress Degradation Behavior of Sulbutiamine HCl

PubMed Central

Farid, Nehal F.; Abdelwahab, Nada S.

2016-01-01

Sulbutiamine (SUL) is an ester of thiazides with neurotropic action. A new stability indicating HPTLC method has been developed and validated for the determination of SUL in the presence of different degradation products. The drug was subjected to different stress conditions following ICH strategy such as hydrolytic degradation (neutral, alkaline and acidic hydrolysis), oxidation, photodegradation and dry heat degradation. The drug demonstrated degradation under all decomposition conditions except neutral hydrolysis and dry heat, where the drug was completely degraded with 0.1 N NaOH, 1 N HCl and 30% H2O2 while it was partially degradaed by 0.1 N HCl, 3% H2O2 and UV light. Structure elucidation of the resulting degradation products was performed using ESI-Q-MS–MS. A well-defined peak for SUL was obtained at Rf = 0.46 and was completely separated from all obtained degradation products. Chromatographic separation was carried out on HPTLC aluminum plates precoated with silica gel 60 F254 using acetone–methylene chloride–ammonia buffer (pH 8.5 ± 0.2) (7:3:0.5, v/v) as a developing system. Densitometric scanning of the separated peaks was performed at 254 nm. System suitability testing parameters were calculated to ascertain the quality performance of the developed method. The method was validated with respect to USP guidelines regarding accuracy, precision, specificity, robustness and ruggedness. Good correlation coefficients were achieved in the range of 0.4–5.0 µg/band, and the limit of detection and limit of quantitation were found to be 0.11 and 0.33 µg/band, respectively. The utility of the suggested method was verified by application to Arcalion forte® tablets where no interference from additives was found. PMID:26759487

Quality by design in the chiral separation strategy for the determination of enantiomeric impurities: development of a capillary electrophoresis method based on dual cyclodextrin systems for the analysis of levosulpiride.

PubMed

Orlandini, S; Pasquini, B; Del Bubba, M; Pinzauti, S; Furlanetto, S

2015-02-06

Quality by design (QbD) concepts, in accordance with International Conference on Harmonisation Pharmaceutical Development guideline Q8(R2), represent an innovative strategy for the development of analytical methods. In this paper QbD principles have been comprehensively applied in the set-up of a capillary electrophoresis method aimed to quantify enantiomeric impurities. The test compound was the chiral drug substance levosulpiride (S-SUL) and the developed method was intended to be used for routine analysis of the pharmaceutical product. The target of analytical QbD approach is to establish a design space (DS) of critical process parameters (CPPs) where the critical quality attributes (CQAs) of the method have been assured to fulfil the desired requirements with a selected probability. QbD can improve the understanding of the enantioseparation process, including both the electrophoretic behavior of enantiomers and their separation, therefore enabling its control. The CQAs were represented by enantioresolution and analysis time. The scouting phase made it possible to select a separation system made by sulfated-β-cyclodextrin and a neutral cyclodextrin, operating in reverse polarity mode. The type of neutral cyclodextrin was included among other CPPs, both instrumental and related to background electrolyte composition, which were evaluated in a screening phase by an asymmetric screening matrix. Response surface methodology was carried out by a Doehlert design and allowed the contour plots to be drawn, highlighting significant interactions between some of the CPPs. DS was defined by applying Monte-Carlo simulations, and corresponded to the following intervals: sulfated-β-cyclodextrin concentration, 9-12 mM; methyl-β-cyclodextrin concentration, 29-38 mM; Britton-Robinson buffer pH, 3.24-3.50; voltage, 12-14 kV. Robustness of the method was examined by a Plackett-Burman matrix and the obtained results, together with system repeatability data, led to define a method control strategy. The method was validated and was finally applied to determine the enantiomeric purity of S-SUL in pharmaceutical dosage forms. Copyright © 2015 Elsevier B.V. All rights reserved.

Response surface methodology for the determination of the design space of enantiomeric separations on cinchona-based zwitterionic chiral stationary phases by high performance liquid chromatography.

PubMed

Hanafi, Rasha Sayed; Lämmerhofer, Michael

2018-01-26

Quality-by-Design approach for enantioselective HPLC method development surpasses Quality-by-Testing in offering the optimal separation conditions with the least number of experiments and in its ability to describe the method's Design Space visually which helps to determine enantiorecognition to a significant extent. Although some schemes exist for enantiomeric separations on Cinchona-based zwitterionic stationary phases, the exact design space and the weights by which each of the chromatographic parameters influences the separation have not yet been statistically studied. In the current work, a screening design followed by a Response Surface Methodology optimization design were adopted for enantioseparation optimization of 3 model drugs namely the acidic Fmoc leucine, the amphoteric tryptophan and the basic salbutamol. The screening design proved that the acid/base additives are of utmost importance for the 3 chiral drugs, and that among 3 different pairs of acids and bases, acetic acid and diethylamine is the couple able to provide acceptable resolution at variable conditions. Visualization of the response surface of the retention factor, separation factor and resolution helped describe accurately the magnitude by which each chromatographic factor (% MeOH, concentration and ratio of acid base modifiers) affects the separation while interacting with other parameters. The global optima compromising highest enantioresolution with the least run time for the 3 chiral model drugs varied extremely, where it was best to set low % methanol with equal ratio of acid-base modifiers for the acidic drug, very high % methanol and 10-fold higher concentration of the acid for the amphoteric drug while 20 folds of the base modifier with moderate %methanol were needed for the basic drug. Considering the selected drugs as models for many series of structurally related compounds, the design space defined and the optimum conditions computed are the key for method development on cinchona-based chiral stationary phases. Copyright © 2017 Elsevier B.V. All rights reserved.

Manufacturing of Proteins and Antibodies: Chapter Downstream Processing Technologies : Harvest Operations.

PubMed

Turner, Richard; Joseph, Adrian; Titchener-Hooker, Nigel; Bender, Jean

2017-08-04

Cell harvesting is the separation or retention of cells and cellular debris from the supernatant containing the target molecule Selection of harvest method strongly depends on the type of cells, mode of bioreactor operation, process scale, and characteristics of the product and cell culture fluid. Most traditional harvesting methods use some form of filtration, centrifugation, or a combination of both for cell separation and/or retention. Filtration methods include normal flow depth filtration and tangential flow microfiltration. The ability to scale down predictably the selected harvest method helps to ensure successful production and is critical for conducting small-scale characterization studies for confirming parameter targets and ranges. In this chapter we describe centrifugation and depth filtration harvesting methods, share strategies for harvest optimization, present recent developments in centrifugation scale-down models, and review alternative harvesting technologies.

Mapping forest inventory and analysis data attributes within the framework of double sampling for stratification design

Treesearch

David C. Chojnacky; Randolph H. Wynne; Christine E. Blinn

2009-01-01

Methodology is lacking to easily map Forest Inventory and Analysis (FIA) inventory statistics for all attribute variables without having to develop separate models and methods for each variable. We developed a mapping method that can directly transfer tabular data to a map on which pixels can be added any way desired to estimate carbon (or any other variable) for a...

Energy Materials Center at Cornell: Final Report

DOE Office of Scientific and Technical Information (OSTI.GOV)

Abruña, Héctor; Mutolo, Paul F

2015-01-02

The mission of the Energy Materials Center at Cornell (emc 2) was to achieve a detailed understanding, via a combination of synthesis of new materials, experimental and computational approaches, of how the nature, structure, and dynamics of nanostructured interfaces affect energy conversion and storage with emphasis on fuel cells, batteries and supercapacitors. Our research on these systems was organized around a full system strategy for; the development and improved performance of materials for both electrodes at which storage or conversion occurs; understanding their internal interfaces, such as SEI layers in batteries and electrocatalyst supports in fuel cells, and methods formore » structuring them to enable high mass transport as well as high ionic and electronic conductivity; development of ion-conducting electrolytes for batteries and fuel cells (separately) and other separator components, as needed; and development of methods for the characterization of these systems under operating conditions (operando methods) Generally, our work took industry and DOE report findings of current materials as a point of departure to focus on novel material sets for improved performance. In addition, some of our work focused on studying existing materials, for example observing battery solvent degradation, fuel cell catalyst coarsening or monitoring lithium dendrite growth, employing in operando methods developed within the center.« less

Fast separation of triterpenoid saponins using supercritical fluid chromatography coupled with single quadrupole mass spectrometry.

PubMed

Huang, Yang; Zhang, Tingting; Zhou, Haibo; Feng, Ying; Fan, Chunlin; Chen, Weijia; Crommen, Jacques; Jiang, Zhengjin

2016-03-20

Triterpenoid saponins (TSs) are the most important components of some traditional Chinese medicines (TCMs) and have exhibited valuable pharmacological properties. In this study, a rapid and efficient method was developed for the separation of kudinosides, stauntosides and ginsenosides using supercritical fluid chromatography coupled with single quadrupole mass spectrometry (SFC-MS). The separation conditions for the selected TSs were carefully optimized after the initial screening of eight stationary phases. The best compromise for all compounds in terms of chromatographic performance and MS sensitivity was obtained when water (5-10%) and formic acid (0.05%) were added to the supercritical carbon dioxide/MeOH mobile phase. Beside the composition of the mobile phase, the nature of the make-up solvent for interfacing SFC with MS was also evaluated. Compared to reversed phase liquid chromatography, the SFC approach showed higher resolution and shorter running time. The developed SFC-MS methods were successfully applied to the separation and identification of TSs present in Ilex latifolia Thunb., Panax quinquefolius L. and Panax ginseng C.A. Meyer. These results suggest that this SFC-MS approach could be employed as a useful tool for the quality assessment of natural products containing TSs as active components. Copyright © 2015 Elsevier B.V. All rights reserved.

Characterization and Separation of Cancer Cells with a Wicking Fiber Device.

PubMed

Tabbaa, Suzanne M; Sharp, Julia L; Burg, Karen J L

2017-12-01

Current cancer diagnostic methods lack the ability to quickly, simply, efficiently, and inexpensively screen cancer cells from a mixed population of cancer and normal cells. Methods based on biomarkers are unreliable due to complexity of cancer cells, plasticity of markers, and lack of common tumorigenic markers. Diagnostics are time intensive, require multiple tests, and provide limited information. In this study, we developed a novel wicking fiber device that separates cancer and normal cell types. To the best of our knowledge, no previous work has used vertical wicking of cells through fibers to identify and isolate cancer cells. The device separated mouse mammary tumor cells from a cellular mixture containing normal mouse mammary cells. Further investigation showed the device separated and isolated human cancer cells from a heterogeneous mixture of normal and cancerous human cells. We report a simple, inexpensive, and rapid technique that has potential to identify and isolate cancer cells from large volumes of liquid samples that can be translated to on-site clinic diagnosis.

Towards a method of rapid extraction of strontium-90 from urine: urine pretreatment and alkali metal removal

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hawkins, C.; Dietz, M.; Kaminski, M.

2016-03-01

A technical program to support the Centers of Disease Control and Prevention is being developed to provide an analytical method for rapid extraction of Sr-90 from urine, with the intent of assessing the general population’s exposure during an emergency response to a radiological terrorist event. Results are presented on the progress in urine sample preparation and chemical separation steps that provide an accurate and quantitative detection of Sr-90 based upon an automated column separation sequence and a liquid scintillation assay. Batch extractions were used to evaluate the urine pretreatment and the column separation efficiency and loading capacity based upon commercial,more » extractant-loaded resins. An efficient pretreatment process for decolorizing and removing organics from urine without measurable loss of radiostrontium from the sample was demonstrated. In addition, the Diphonix® resin shows promise for the removal of high concentrations of common strontium interferents in urine as a first separation step for Sr-90 analysis.« less

Microchip electrophoresis with electrochemical detection for the determination of analytes in the dopamine metabolic pathway

PubMed Central

Saylor, Rachel A.; Reid, Erin A.; Lunte, Susan M.

2016-01-01

A method for the separation and detection of analytes in the dopamine metabolic pathway was developed using microchip electrophoresis with electrochemical detection. The microchip consisted of a 5 cm PDMS separation channel in a simple-t configuration. Analytes in the dopamine metabolic pathway were separated using a background electrolyte composed of 15 mM phosphate at pH 7.4, 15 mM SDS, and 2.5 mM boric acid. Two different microchip substrates using different electrode materials were compared for the analysis: a PDMS/PDMS device with a carbon fiber electrode and a PDMS/glass hybrid device with a pyrolyzed photoresist film carbon electrode. While the PDMS/PDMS device generated high separation efficiencies and good resolution, more reproducible migration times were obtained with the PDMS/glass hybrid device, making it a better choice for biological applications. Lastly, the optimized method was used to monitor L-DOPA metabolism in a rat brain slice. PMID:25958983

Study on Separation of Structural Isomer with Magneto-Archimedes method

NASA Astrophysics Data System (ADS)

Kobayashi, T.; Mori, T.; Akiyama, Y.; Mishima, F.; Nishijima, S.

2017-09-01

Organic compounds are refined by separating their structural isomers, however each separation method has some problems. For example, distillation consumes large energy. In order to solve these problems, new separation method is needed. Considering organic compounds are diamagnetic, we focused on magneto-Archimedes method. With this method, particle mixture dispersed in a paramagnetic medium can be separated in a magnetic field due to the difference of the density and magnetic susceptibility of the particles. In this study, we succeeded in separating isomers of phthalic acid as an example of structural isomer using MnCl2 solution as the paramagnetic medium. In order to use magneto-Archimedes method for separating materials for food or medicine, we proposed harmless medium using oxygen and fluorocarbon instead of MnCl2 aqueous solution. As a result, the possibility of separating every structural isomer was shown.

A novel tertiary prep-HPLC method for the isolation of single amino acids for AMS-radiocarbon measurement.

PubMed

Fernandes, Ricardo; Koudelka, Tomas; Tholey, Andreas; Dreves, Alexander

2017-07-15

AMS-radiocarbon measurements of amino acids can potentially provide more reliable radiocarbon dates than bulk collagen analysis. Nonetheless, the applicability of such an approach is often limited by the low-throughput of existing isolation methods and difficulties in determining the contamination introduced during the separation process. A novel tertiary prep-HPLC amino acid isolation method was developed that relies on the combustion of eluted material without requiring any additional chemical steps. Amino acid separation was carried out using a gradient mix of pure water and phosphoric acid with an acetonitrile step in-between runs to remove hydrophobic molecules from the separation column. The amount of contaminant carbon and its 14 C content were determined from two-point measurements of collagen samples of known 14 C content. The amount of foreign carbon due to the isolation process was estimated at 4±1μg and its 14 C content was 0.43±0.01 F 14 C. Radiocarbon values corrected for carbon contamination have only a minor increase in uncertainties. For Holocene samples, this corresponds to an added uncertainty typically smaller than 10 14 Cyears. The developed method can be added to routine AMS measurements without implying significant operational changes and offers a level of measurement uncertainty that is suitable for many archaeological, ecological, environmental, and biological applications. Copyright © 2017. Published by Elsevier B.V.

Unexpected retention behavior of baicalin: Hydrophilic interaction like properties of a reversed-phase column.

PubMed

Magda, Balázs; Márta, Zoltán; Imre, Tímea; Kalapos-Kovács, Bernadett; Klebovich, Imre; Fekete, Jenő; Szabó, Pál T

2015-01-01

The original aim of this study was to develop a method for the determination of baicalin from membrane vesicles. The unconventional chromatographic separation ("inverse gradient elution" on a reversed phase column) was due to a lucky chance, which is detailed and discussed in this study. The validated liquid chromatography-tandem mass spectrometry (LC-MS/MS) method is proved to be sensitive, rapid and selective. Chromatographic separation was performed on a Zorbax SB-C8 column (250 mm × 4.6 mm, i.d.; 5 μm) with 0.1% formic acid in water and methanol by linear gradient elution. Quantification of baicalin was determined by multiple reaction monitoring (MRM) mode using electrospray ionization (ESI). The calibration curve was linear (r = 0.9987) over the concentration range from 1 to 1000 nM. The coefficient of variation and relative error of baicalin for intra- and inter-assay at three quality control (QC) levels were 2.0-10.2% and -6.1 to 6.7%, respectively. The lower limit of quantification (LLOQ) for baicalin was 1 nM (0.446 ng/ml), without preconcentration of the sample. This method was subsequently applied to vesicular transport assays of baicalin in membrane vesicles successfully. The developed method can open up new area of research in the chromatographic separation of flavonoids and their glucuronides. Copyright © 2015. Published by Elsevier B.V.

(PRESENT AT NCCU) ANALYSIS OF SELECTED PYRETHROID PESTICIDES USING REVERSE PHASE HIGH LIQUID CHROMATOGRAPHY

EPA Science Inventory

This research was conducted in cooperation with EPA Region 4 in Athens, GA to develop a method to analyze selected pyrethroid pesticides using Reverse Phase-High Pressure Liquid Chromatography (HPLC). This HPLC method will aid researchers in separating and identifying these pyre...

Feature selection methods for object-based classification of sub-decimeter resolution digital aerial imagery

USDA-ARS?s Scientific Manuscript database

Due to the availability of numerous spectral, spatial, and contextual features, the determination of optimal features and class separabilities can be a time consuming process in object-based image analysis (OBIA). While several feature selection methods have been developed to assist OBIA, a robust c...

Simultaneous analysis of nucleobases, nucleosides and ginsenosides in ginseng extracts using supercritical fluid chromatography coupled with single quadrupole mass spectrometry.

PubMed

Huang, Yang; Zhang, Tingting; Zhao, Yumei; Zhou, Haibo; Tang, Guangyun; Fillet, Marianne; Crommen, Jacques; Jiang, Zhengjin

2017-09-10

Nucleobases, nucleosides and ginsenosides, which have a significant impact on the physiological activity of organisms, are reported to be the active components of ginseng, while they are less present in ginseng extracts. Few analytical methods have been developed so far to simultaneously analyze these three classes of compounds with different polarities present in ginseng extracts. In the present study, a simple and efficient analytical method was successfully developed for the simultaneous separation of 17 nucleobases, nucleosides and ginsenosides in ginseng extracts using supercritical fluid chromatography coupled with single quadrupole mass spectrometry (SFC-MS). The effect of various experimental factors on the separation performance, such as the column type, temperature and backpressure, the type of modifier and additive, and the concentration of make-up solvent were systematically investigated. Under the selected conditions, the developed method was successfully applied to the quality evaluation of 14 batches of ginseng extracts from different origins. The results obtained for the different batches indicate that this method could be employed for the quality assessment of ginseng extracts. Copyright © 2017 Elsevier B.V. All rights reserved.

Validated enantiospecific LC method for determination of (R)-enantiomer impurity in (S)-efavirenz.

PubMed

Seshachalam, U; Narasimha Rao, D V L; Chandrasekhar, K B

2008-02-01

A high-performance liquid chromatographic method was developed for separation of the enantiomers of efavirenz. The developed method was applied for the determination of (R)-enantiomer in (S)-efavirenz and satisfactory results were achieved. The base line separation with a resolution of more than 4.0 was achieved on Chiralcel OD (250 mm x 4.6 mm, 10 microm) column containing tris-(3,5-dimethylphenylcarbomate) as stationary phase. The mobile phase consists of n-hexane: isopropyl alcohol (80:20 v/v) with 0.1% (v/v) of formic acid as additive. The flow rate was kept at 1.0 ml/min and the UV detection was monitored at 254 nm. The (R)-enantiomer was found linear over the range of 0.1 microg/ml--6 microg/ml. The limit of detection (LOD) was 0.03 microg/ml and the limit of quantification (LOQ) was 0.1 microg/ml (n=3. The precision of (R)-enantiomer at LOQ level was evaluated through six replicate injections and the RSD of the peak response was achieved as 1.34%. The results demonstrated that the developed LC method was simple, precise, robust and applicable for the purity determination of efavirenz.

PHARMACEUTICAL AND BIOMEDICAL APPLICATIONS OF AFFINITY CHROMATOGRAPHY: RECENT TRENDS AND DEVELOPMENTS

PubMed Central

Hage, David S.; Anguizola, Jeanethe A.; Bi, Cong; Li, Rong; Matsuda, Ryan; Papastavros, Efthimia; Pfaunmiller, Erika; Vargas, John; Zheng, Xiwei

2012-01-01

Affinity chromatography is a separation technique that has become increasingly important in work with biological samples and pharmaceutical agents. This method is based on the use of a biologically-related agent as a stationary phase to selectively retain analytes or to study biological interactions. This review discusses the basic principles behind affinity chromatography and examines recent developments that have occurred in the use of this method for biomedical and pharmaceutical analysis. Techniques based on traditional affinity supports are discussed, but an emphasis is placed on methods in which affinity columns are used as part of HPLC systems or in combination with other analytical methods. General formats for affinity chromatography that are considered include step elution schemes, weak affinity chromatography, affinity extraction and affinity depletion. Specific separation techniques that are examined include lectin affinity chromatography, boronate affinity chromatography, immunoaffinity chromatography, and immobilized metal ion affinity chromatography. Approaches for the study of biological interactions by affinity chromatography are also presented, such as the measurement of equilibrium constants, rate constants, or competition and displacement effects. In addition, related developments in the use of immobilized enzyme reactors, molecularly imprinted polymers, dye ligands and aptamers are briefly considered. PMID:22305083

Optimization of capillary zone electrophoresis for charge heterogeneity testing of biopharmaceuticals using enhanced method development principles.

PubMed

Moritz, Bernd; Locatelli, Valentina; Niess, Michele; Bathke, Andrea; Kiessig, Steffen; Entler, Barbara; Finkler, Christof; Wegele, Harald; Stracke, Jan

2017-12-01

CZE is a well-established technique for charge heterogeneity testing of biopharmaceuticals. It is based on the differences between the ratios of net charge and hydrodynamic radius. In an extensive intercompany study, it was recently shown that CZE is very robust and can be easily implemented in labs that did not perform it before. However, individual characteristics of some examined proteins resulted in suboptimal resolution. Therefore, enhanced method development principles were applied here to investigate possibilities for further method optimization. For this purpose, a high number of different method parameters was evaluated with the aim to improve CZE separation. For the relevant parameters, design of experiments (DoE) models were generated and optimized in several ways for different sets of responses like resolution, peak width and number of peaks. In spite of product specific DoE optimization it was found that the resulting combination of optimized parameters did result in significant improvement of separation for 13 out of 16 different antibodies and other molecule formats. These results clearly demonstrate generic applicability of the optimized CZE method. Adaptation to individual molecular properties may sometimes still be required in order to achieve optimal separation but the set screws discussed in this study [mainly pH, identity of the polymer additive (HPC versus HPMC) and the concentrations of additives like acetonitrile, butanolamine and TETA] are expected to significantly reduce the effort for specific optimization. 2017 The Authors. Electrophoresis published by Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Systematic Development and Validation of a Thin-Layer Densitometric Bioanalytical Method for Estimation of Mangiferin Employing Analytical Quality by Design (AQbD) Approach

PubMed Central

Khurana, Rajneet Kaur; Rao, Satish; Beg, Sarwar; Katare, O.P.; Singh, Bhupinder

2016-01-01

The present work aims at the systematic development of a simple, rapid and highly sensitive densitometry-based thin-layer chromatographic method for the quantification of mangiferin in bioanalytical samples. Initially, the quality target method profile was defined and critical analytical attributes (CAAs) earmarked, namely, retardation factor (Rf), peak height, capacity factor, theoretical plates and separation number. Face-centered cubic design was selected for optimization of volume loaded and plate dimensions as the critical method parameters selected from screening studies employing D-optimal and Plackett–Burman design studies, followed by evaluating their effect on the CAAs. The mobile phase containing a mixture of ethyl acetate : acetic acid : formic acid : water in a 7 : 1 : 1 : 1 (v/v/v/v) ratio was finally selected as the optimized solvent for apt chromatographic separation of mangiferin at 262 nm with Rf 0.68 ± 0.02 and all other parameters within the acceptance limits. Method validation studies revealed high linearity in the concentration range of 50–800 ng/band for mangiferin. The developed method showed high accuracy, precision, ruggedness, robustness, specificity, sensitivity, selectivity and recovery. In a nutshell, the bioanalytical method for analysis of mangiferin in plasma revealed the presence of well-resolved peaks and high recovery of mangiferin. PMID:26912808

Analytical investigation of aerodynamic characteristics of highly swept wings with separated flow

NASA Technical Reports Server (NTRS)

Reddy, C. S.

1980-01-01

Many modern aircraft designed for supersonic speeds employ highly swept-back and low-aspect-ratio wings with sharp or thin edges. Flow separation occurs near the leading and tip edges of such wings at moderate to high angles of attack. Attempts have been made over the years to develop analytical methods for predicting the aerodynamic characteristics of such aircraft. Before any method can really be useful, it must be tested against a standard set of data to determine its capabilities and limitations. The present work undertakes such an investigation. Three methods are considered: the free-vortex-sheet method (Weber et al., 1975), the vortex-lattice method with suction analogy (Lamar and Gloss, 1975), and the quasi-vortex lattice method of Mehrotra (1977). Both flat and cambered wings of different configurations, for which experimental data are available, are studied and comparisons made.

Developing a system for blind acoustic source localization and separation

NASA Astrophysics Data System (ADS)

Kulkarni, Raghavendra

This dissertation presents innovate methodologies for locating, extracting, and separating multiple incoherent sound sources in three-dimensional (3D) space; and applications of the time reversal (TR) algorithm to pinpoint the hyper active neural activities inside the brain auditory structure that are correlated to the tinnitus pathology. Specifically, an acoustic modeling based method is developed for locating arbitrary and incoherent sound sources in 3D space in real time by using a minimal number of microphones, and the Point Source Separation (PSS) method is developed for extracting target signals from directly measured mixed signals. Combining these two approaches leads to a novel technology known as Blind Sources Localization and Separation (BSLS) that enables one to locate multiple incoherent sound signals in 3D space and separate original individual sources simultaneously, based on the directly measured mixed signals. These technologies have been validated through numerical simulations and experiments conducted in various non-ideal environments where there are non-negligible, unspecified sound reflections and reverberation as well as interferences from random background noise. Another innovation presented in this dissertation is concerned with applications of the TR algorithm to pinpoint the exact locations of hyper-active neurons in the brain auditory structure that are directly correlated to the tinnitus perception. Benchmark tests conducted on normal rats have confirmed the localization results provided by the TR algorithm. Results demonstrate that the spatial resolution of this source localization can be as high as the micrometer level. This high precision localization may lead to a paradigm shift in tinnitus diagnosis, which may in turn produce a more cost-effective treatment for tinnitus than any of the existing ones.

Facile Separation of 5-O-Galloylquinic Acid from Chinese Green Tea Extract using Mesoporous Zirconium Phosphate.

PubMed

Ma, Yilong; Shang, Yafang; Zhu, Danye; Wang, Caihong; Zhong, Zhifeng; Xu, Ziyang

2016-05-01

5-O-Galloylquinic acid from green tea and other plants is attracting increasing attention for its antioxidant and antileishmanial bioactivities. It is always isolated using a silica column, a Sephadex column and high-performance liquid chromatography (HPLC) methods, which are either laborious or instrument dependent. To develop a new method to easily separate 5-O-galloylquinic acid. Mesoporous zirconium phosphate (m-ZrP) was prepared to conveniently separate 5-O-galloylquinic acid from Chinese green tea extract, and the target compound was easily obtained by simple steps of adsorption, washing and desorption. The effects of the green tea extraction conditions, extract concentrations, and m-ZrP adsorption/desorption dynamics on the 5-O-galloylquinic acid separation were evaluated. 5-O-Galloylquinic acid that was separated from a 70% ethanol extract of green tea was of moderate HPLC purity (92%) and recovery (88%), and an increased non-specific binding of epigallocatechin gallate (EGCG) on m-ZrP was observed in the diluted tea extract. The times for maximal adsorption of 5-O-galloylquinic acid in 70% ethanol extract and maximal desorption of 5-O-galloylquinic acid in 0.4% phosphoric acid solution were confirmed as 7 h and 5 h, respectively. A facile method to separate 5-O-galloylquinic acid from Chinese green tea extract using m-ZrP was established. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Centrifugal partition chromatography: A preparative tool for isolation and purification of xylindein from Chlorociboria aeruginosa.

PubMed

Boonloed, Anukul; Weber, Genevieve L; Ramzy, Kelly M; Dias, Veronica R; Remcho, Vincent T

2016-12-23

A centrifugal partition chromatography (CPC) method was developed for the preparative-scale isolation and purification of xylindein from the wood-staining fungi, Chlorociboria aeruginosa. Xylindein, a blue-green pigment naturally secreted from the hyphae and fruiting bodies of the fungus, has great value in the decorative wood industry and textile coloration. Xylindein has great potential for use as a fluorescent labeling agent as well as in organic semiconductor applications. However, a primary limitation of xylindein is its poor solubility in most common HPLC solvents. Consequently, it is arduous to purify using preparative liquid chromatography or solid-phase extraction (SPE). Support-free, liquid-liquid chromatographic methods, including CPC, where solutes are separated based on their different distribution coefficients (K D ) between two immiscible solvent systems, are promising alternatives for the purification of the compound on a preparative scale. In this work, a new biphasic solvent system suitable for CPC separation of xylindein was developed. Various groups of solvents were assessed for their suitability as xylindein extractants. A new solvent system suitable for CPC separation of xylindein, composed of heptane/THF/MEK/acetonitrile/acetic acid/water, was developed. This solvent system yielded a K D value for xylindein of 1.54±0.04, as determined by HPLC (n=3). The compositions of the upper phase and lower phase of the solvent system were determined by Heteronuclear Single Quantum Correlation (HSQC) NMR and proton NMR. A CPC system, equipped with a fraction collector, was used for the isolation of xylindein from crude extracts. The xylindein fractions isolated by the CPC were then analyzed using HPLC and presented as a fractogram. Based on the CPC fractogram, the purified xylindein fractions were achieved after 30min CPC separation time, yielding 71% extraction efficiency. The developed CPC method allowed for isolation of this naturally sourced xylindein in amounts suitable for further study. Copyright © 2016 Elsevier B.V. All rights reserved.

Automated total and radioactive strontium separation and preconcentration in samples of environmental interest exploiting a lab-on-valve system.

PubMed

Rodríguez, Rogelio; Avivar, Jessica; Ferrer, Laura; Leal, Luz O; Cerdà, Victor

2012-07-15

A novel lab-on-valve system has been developed for strontium determination in environmental samples. Miniaturized lab-on-valve system potentially offers facilities to allow any kind of chemical and physical processes, including fluidic and microcarrier bead control, homogenous reaction and liquid-solid interaction. A rapid, inexpensive and fully automated method for the separation and preconcentration of total and radioactive strontium, using a solid phase extraction material (Sr-Resin), has been developed. Total strontium concentrations are determined by ICP-OES and (90)Sr activities by a low background proportional counter. The method has been successfully applied to different water samples of environmental interest. The proposed system offers minimization of sample handling, drastic reduction of reagent volume, improvement of the reproducibility and sample throughput and attains a significant decrease of both time and cost per analysis. The LLD of the total Sr reached is 1.8ng and the minimum detectable activity for (90)Sr is 0.008Bq. The repeatability of the separation procedure is 1.2% (n=10). Copyright © 2011 Elsevier B.V. All rights reserved.

Failure analysis of pinch-torsion tests as a thermal runaway risk evaluation method of Li-ion cells

NASA Astrophysics Data System (ADS)

Xia, Yuzhi; Li, Tianlei; Ren, Fei; Gao, Yanfei; Wang, Hsin

2014-11-01

Recently a pinch-torsion test is developed for safety testing of Li-ion batteries. It has been demonstrated that this test can generate small internal short-circuit spots in the separator in a controllable and repeatable manner. In the current research, the failure mechanism is examined by numerical simulations and comparisons to experimental observations. Finite element models are developed to evaluate the deformation of the separators under both pure pinch and pinch-torsion loading conditions. It is discovered that the addition of the torsion component significantly increased the maximum first principal strain, which is believed to induce the internal short circuit. In addition, the applied load in the pinch-torsion test is significantly less than in the pure pinch test, thus dramatically improving the applicability of this method to ultra-thick batteries which otherwise require heavy load in excess of machine capability. It is further found that the separator failure is achieved in the early stage of torsion (within a few degree of rotation). Effect of coefficient of friction on the maximum first principal strain is also examined.

Pressurized capillary electrochromatographic analysis of water-soluble vitamins by combining with on-line concentration technique.

PubMed

Jia, Li; Liu, Yaling; Du, Yanyan; Xing, Da

2007-06-22

A pressurized capillary electrochromatography (pCEC) system was developed for the separation of water-soluble vitamins, in which UV absorbance was used as the detection method and a monolithic silica-ODS column as the separation column. The parameters (type and content of organic solvent in the mobile phase, type and concentration of electrolyte, pH of the electrolyte buffer, applied voltage and flow rate) affecting the separation resolution were evaluated. The combination of two on-line concentration techniques, namely, solvent gradient zone sharpening effect and field-enhanced sample stacking, was utilized to improve detection sensitivity, which proved to be beneficial to enhance the detection sensitivity by enabling the injection of large volumes of samples. Coupling electrokinetic injection with the on-line concentration techniques was much more beneficial for the concentration of positively charged vitamins. Comparing with the conventional injection mode, the enhancement in the detection sensitivities of water-soluble vitamins using the on-line concentration technique is in the range of 3 to 35-fold. The developed pCEC method was applied to evaluate water-soluble vitamins in corns.

Quantitation of 11 alkylamines in atmospheric samples: separating structural isomers by ion chromatography

NASA Astrophysics Data System (ADS)

Place, Bryan K.; Quilty, Aleya T.; Di Lorenzo, Robert A.; Ziegler, Susan E.; VandenBoer, Trevor C.

2017-03-01

Amines are important drivers in particle formation and growth, which have implications for Earth's climate. In this work, we developed an ion chromatographic (IC) method using sample cation-exchange preconcentration for separating and quantifying the nine most abundant atmospheric alkylamines (monomethylamine (MMAH+), dimethylamine (DMAH+), trimethylamine (TMAH+), monoethylamine (MEAH+), diethylamine (DEAH+), triethylamine (TEAH+), monopropylamine (MPAH+), isomonopropylamine (iMPAH+), and monobutylamine (MBAH+)) and two alkyl diamines (1, 4-diaminobutane (DABH+) and 1, 5-diaminopentane (DAPH+)). Further, the developed method separates the suite of amines from five common atmospheric inorganic cations (Na+, NH4+, K+, Mg2+, Ca2+). All 16 cations are greater than 95 % baseline resolved and elute in a runtime of 35 min. This paper describes the first successful separation of DEAH+ and TMAH+ by IC and achieves separation between three sets of structural isomers, providing specificity not possible by mass spectrometry. The method detection limits for the alkylamines are in the picogram per injection range and the method precision (±1σ) analyzed over 3 months was within 16 % for all the cations. The performance of the IC method for atmospheric application was tested with biomass-burning (BB) particle extracts collected from two forest fire plumes in Canada. In extracts of a size-resolved BB sample from an aged plume, we detected and quantified MMAH+, DMAH+, TMAH+, MEAH+, DEAH+, and TEAH+ in the presence of Na+, NH4+, and K+ at molar ratios of amine to inorganic cation ranging from 1 : 2 to 1 : 1000. Quantities of DEAH+ and DMAH+ of 0.2-200 and 3-1200 ng m-3, respectively, were present in the extracts and an unprecedented amine-to-ammonium molar ratio greater than 1 was observed in particles with diameters spanning 56-180 nm. Extracts of respirable fine-mode particles (PM2. 5) from a summer forest fire in British Columbia in 2015 were found to contain iMPAH+, TMAH+, DEAH+ and TEAH+ at molar ratios of 1 : 300 with the dominant cations. The amine-to-ammonium ratio in a time series of samples never exceeded 0.15 during the sampling of the plume. These results and an amine standard addition demonstrate the robustness and sensitivity of the developed method when applied to the complex matrix of BB particle samples. The detection of multiple alkylamines in the analyzed BB samples indicates that this speciation and quantitation approach can be used to constrain BB emission estimates and the biogeochemical cycling of these reduced nitrogen species.

Separation of 20 coumarin derivatives using the capillary electrophoresis method optimized by a series of Doehlert experimental designs.

PubMed

Woźniakiewicz, Michał; Gładysz, Marta; Nowak, Paweł M; Kędzior, Justyna; Kościelniak, Paweł

2017-05-15

The aim of this study was to develop the first CE-based method enabling separation of 20 structurally similar coumarin derivatives. To facilitate method optimization a series of three consequent Doehlert experimental designs with the response surface methodology was employed, using number of peaks and the adjusted time of analysis as the selected responses. Initially, three variables were examined: buffer pH, ionic strength and temperature (No. 1 Doehlert design). The optimal conditions provided only partial separation, on that account, several buffer additives were examined at the next step: organic cosolvents and cyclodextrin (No. 2 Doehlert design). The optimal cyclodextrin type was also selected experimentally. The most promising results were obtained for the buffers fortified with methanol, acetonitrile and heptakis(2,3,6-tri-O-methyl)-β-cyclodextrin. Since these additives may potentially affect acid-base equilibrium and ionization state of analytes, the third Doehlert design (No. 3) was used to reconcile concentration of these additives with optimal pH. Ultimately, the total separation of all 20 compounds was achieved using the borate buffer at basic pH 9.5 in the presence of 10mM cyclodextrin, 9% (v/v) acetonitrile and 36% (v/v) methanol. Identity of all compounds was confirmed using the in-lab build UV-VIS spectra library. The developed method succeeded in identification of coumarin derivatives in three real samples. It demonstrates a huge resolving power of CE assisted by addition of cyclodextrins and organic cosolvents. Our unique optimization approach, based on the three Doehlert designs, seems to be prospective for future applications of this technique. Copyright © 2017 Elsevier B.V. All rights reserved.

Analysis of glycosaminoglycan-derived disaccharides by capillary electrophoresis using laser-induced fluorescence detection

PubMed Central

Chang, Yuqing; Yang, Bo; Zhao, Xue; Linhardt, Robert J.

2012-01-01

A quantitative and highly sensitive method for the analysis of glycosaminoglycan (GAG)-derived disaccharides is presented that relies on capillary electrophoresis (CE) with laser-induced fluorescence (LIF) detection. This method enables complete separation of seventeen GAG-derived disaccharides in a single run. Unsaturated disaccharides were derivatized with 2-aminoacridone (AMAC) to improve sensitivity. The limit of detection was at the attomole level and about 100-fold more sensitive than traditional CE-ultraviolet detection. A CE separation timetable was developed to achieve complete resolution and shorten analysis time. The RSD of migration time and peak areas at both low and high concentrations of unsaturated disaccharides are all less than 2.7% and 3.2%, respectively, demonstrating that this is a reproducible method. This analysis was successfully applied to cultured Chinese hamster ovary cell samples for determination of GAG disaccharides. The current method simplifies GAG extraction steps, and reduces inaccuracy in calculating ratios of heparin/heparan sulfate to chondroitin sulfate/dermatan sulfate, resulting from the separate analyses of a single sample. PMID:22609076

"Inject-mix-react-separate-and-quantitate" (IMReSQ) method for screening enzyme inhibitors.

PubMed

Wong, Edmund; Okhonin, Victor; Berezovski, Maxim V; Nozaki, Tomoyoshi; Waldmann, Herbert; Alexandrov, Kirill; Krylov, Sergey N

2008-09-10

Many regulatory enzymes are considered attractive therapeutic targets, and their inhibitors are potential drug candidates. Screening combinatorial libraries for enzyme inhibitors is pivotal to identifying hit compounds for the development of drugs targeting regulatory enzymes. Here, we introduce the first inhibitor screening method that consumes only nanoliters of the reactant solutions and is applicable to regulatory enzymes. The method is termed inject-mix-react-separate-and-quantitate (IMReSQ) and includes five steps. First, nanoliter volumes of substrate, candidate inhibitor, and enzyme solutions are injected by pressure into a capillary as separate plugs. Second, the plugs are mixed inside this capillary microreactor by transverse diffusion of laminar flow profiles. Third, the reaction mixture is incubated to form the enzymatic product. Fourth, the product is separated from the substrate inside the capillary by electrophoresis. Fifth, the amounts of the product and substrate are quantitated. In this proof-of-principle work, we applied IMReSQ to study inhibition of recently cloned protein farnesyltransferase from parasite Entamoeba histolytica. This enzyme is a potential therapeutic target for antiparasitic drugs. We identified three previously unknown inhibitors of this enzyme and proved that IMReSQ could be used for quantitatively ranking the potencies of inhibitors.

Rapid and Convenient Separation of Chitooligosaccharides by Ion-Exchange Chromatography

NASA Astrophysics Data System (ADS)

Wu, Yuxiao; Lu, Wei-Peng; Wang, Jianing; Gao, Yunhua; Guo, Yanchuan

2017-12-01

Pervious methods for separation of highly purified chitooligosaccharides was time-consuming and labor-intensive, which limited the large-scale production. This study developed a convenient ion-exchange chromatography using the ÄKTA™ avant 150 chromatographic system. Five fractions were automatically collected under detecting the absorption at 210 nm. The fractions were analyzed by high-performance liquid chromatography. It proved that they primarily comprised chitobiose, chitotriose, chitotetraose, chitopentaose, and chitohexaose, respectively, with chromatographic purities over 90%. The separation process was rapid, convenient and could be monitored on-line, which would be benefit for the mass production of chitooligosaccharides.

[Advancements of computer chemistry in separation of Chinese medicine].

PubMed

Li, Lingjuan; Hong, Hong; Xu, Xuesong; Guo, Liwei

2011-12-01

Separating technique of Chinese medicine is not only a key technique in the field of Chinese medicine' s research and development, but also a significant step in the modernization of Chinese medicinal preparation. Computer chemistry can build model and look for the regulations from Chinese medicine system which is full of complicated data. This paper analyzed the applicability, key technology, basic mode and common algorithm of computer chemistry applied in the separation of Chinese medicine, introduced the mathematic mode and the setting methods of Extraction kinetics, investigated several problems which based on traditional Chinese medicine membrane procession, and forecasted the application prospect.

Separation of antibody drug conjugate species by RPLC: A generic method development approach.

PubMed

Fekete, Szabolcs; Molnár, Imre; Guillarme, Davy

2017-04-15

This study reports the use of modelling software for the successful method development of IgG1 cysteine conjugated antibody drug conjugate (ADC) in RPLC. The goal of such a method is to be able to calculate the average drug to antibody ratio (DAR) of and ADC product. A generic method development strategy was proposed including the optimization of mobile phase temperature, gradient profile and mobile phase ternary composition. For the first time, a 3D retention modelling was presented for large therapeutic protein. Based on a limited number of preliminary experiments, a fast and efficient separation of the DAR species of a commercial ADC sample, namely brentuximab vedotin, was achieved. The prediction offered by the retention model was found to be highly reliable, with an average error of retention time prediction always lower than 0.5% using a 2D or 3D retention models. For routine purpose, four to six initial experiments were required to build the 2D retention models, while 12 experiments were recommended to create the 3D model. At the end, RPLC can therefore be considered as a good method for estimating the average DAR of an ADC, based on the observed peak area ratios of RPLC chromatogram of the reduced ADC sample. Copyright © 2017 Elsevier B.V. All rights reserved.

A validated stability indicating RP-HPLC method for estimation of Armodafinil in pharmaceutical dosage forms and characterization of its base hydrolytic product.

PubMed

Venkateswarlu, Kambham; Rangareddy, Ardhgeri; Narasimhaiah, Kanaka; Sharma, Hemraj; Bandi, Naga Mallikarjuna Raja

2017-01-01

The main objective of present study was to develop a RP-HPLC method for estimation of Armodafinil in pharmaceutical dosage forms and characterization of its base hydrolytic product. The method was developed for Armodafinil estimation and base hydrolytic products were characterized. The separation was carried out on C18 column by using mobile phase as mixture of water and methanol (45:55%v/v). Eluents were detected at 220nm at 1ml/min. Stress studies were performed with milder conditions followed by stronger conditions so as to get sufficient degradation around 20%. A total of five degradation products were detected and separated from analyte. The linearity of the proposed method was investigated in the range of 20-120µg/ml for Armodafinil. The detection limit and quantification limit was found to be 0.01183μg/ml and 0.035µg/ml respectively. The precision % RSD was found to be less than 2% and the recovery was between 98-102%. Armodafinil was found to be more sensitive to the base hydrolysis and yielded its carboxylic acid as degradant. The developed method was stability indicating assay, suitable to quantify Armodafinil in presence of possible degradants. The drug was sensitive to acid, base &photolytic stress and resistant to thermal &oxidation.

Automated statistical experimental design approach for rapid separation of coenzyme Q10 and identification of its biotechnological process related impurities using UHPLC and UHPLC-APCI-MS.

PubMed

Talluri, Murali V N Kumar; Kalariya, Pradipbhai D; Dharavath, Shireesha; Shaikh, Naeem; Garg, Prabha; Ramisetti, Nageswara Rao; Ragampeta, Srinivas

2016-09-01

A novel ultra high performance liquid chromatography method development strategy was ameliorated by applying quality by design approach. The developed systematic approach was divided into five steps (i) Analytical Target Profile, (ii) Critical Quality Attributes, (iii) Risk Assessments of Critical parameters using design of experiments (screening and optimization phases), (iv) Generation of design space, and (v) Process Capability Analysis (Cp) for robustness study using Monte Carlo simulation. The complete quality-by-design-based method development was made automated and expedited by employing sub-2 μm particles column with an ultra high performance liquid chromatography system. Successful chromatographic separation of the Coenzyme Q10 from its biotechnological process related impurities was achieved on a Waters Acquity phenyl hexyl (100 mm × 2.1 mm, 1.7 μm) column with gradient elution of 10 mM ammonium acetate buffer (pH 4.0) and a mixture of acetonitrile/2-propanol (1:1) as the mobile phase. Through this study, fast and organized method development workflow was developed and robustness of the method was also demonstrated. The method was validated for specificity, linearity, accuracy, precision, and robustness in compliance to the International Conference on Harmonization, Q2 (R1) guidelines. The impurities were identified by atmospheric pressure chemical ionization-mass spectrometry technique. Further, the in silico toxicity of impurities was analyzed using TOPKAT and DEREK software. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

On-line comprehensive two-dimensional normal-phase liquid chromatography × reversed-phase liquid chromatography for preparative isolation of Peucedanum praeruptorum.

PubMed

Wang, Xin-Yuan; Li, Jia-Fu; Jian, Ya-Mei; Wu, Zhen; Fang, Mei-Juan; Qiu, Ying-Kun

2015-03-27

A new on-line comprehensive preparative two-dimensional normal-phase liquid chromatography × reversed-phase liquid chromatography (2D NPLC × RPLC) system was developed for the separation of complicated natural products. It was based on the use of a silica gel packed medium-pressure column as the first dimension and an ODS preparative HPLC column as the second dimension. The two dimensions were connected with normal-phase (NP) and reversed-phase (RP) enrichment units, involving a newly developed airflow assisted adsorption (AAA) technique. The instrument operation and the performance of this NPLC × RPLC separation method were illustrated by gram-scale isolation of ethanol extract from the roots of Peucedanum praeruptorum. In total, 19 compounds with high purity were obtained via automated multi-step preparative separation in a short period of time using this system, and their structures were comprehensively characterized by ESI-MS, (1)H NMR, and (13)C NMR. Including two new compounds, five isomers in two groups with identical HPLC and TLC retention values were also obtained and identified by 1D NMR and 2D NMR. This is the first report of an NPLC × RPLC system successfully applied in an on-line preparative process. This system not only solved the interfacing problem of mobile-phase immiscibility caused by NP and RP separation, it also exhibited apparent advantages in separation efficiency and sample treatment capacity compared with conventional methods. Copyright © 2015 Elsevier B.V. All rights reserved.

Studies on separation and purification of fission (99)Mo from neutron activated uranium aluminum alloy.

PubMed

Rao, Ankita; Kumar Sharma, Abhishek; Kumar, Pradeep; Charyulu, M M; Tomar, B S; Ramakumar, K L

2014-07-01

A new method has been developed for separation and purification of fission (99)Mo from neutron activated uranium-aluminum alloy. Alkali dissolution of the irradiated target (100mg) results in aluminum along with (99)Mo and a few fission products passing into solution, while most of the fission products, activation products and uranium remain undissolved. Subsequent purification steps involve precipitation of aluminum as Al(OH)3, iodine as AgI/AgIO3 and molybdenum as Mo-α-benzoin oxime. Ruthenium is separated by volatilization as RuO4 and final purification of (99)Mo was carried out using anion exchange method. The radiochemical yield of fission (99)Mo was found to be >80% and the purity of the product was in conformity with the international pharmacopoeia standards. Copyright © 2014 Elsevier Ltd. All rights reserved.

Paired-ion chromatography and high performance liquid chromatography of labetalol in feeds.

PubMed

Townley, E R; Ross, B

1980-11-01

A high performance liquid chromatographic (HPLC) method using reverse phase paired-ion chromatography and ultraviolet detection at 280 nm has been developed to determine labetalol, an alpha and beta adrenoceptor blocking agent, in Purina No. 5001 rodent chow. The method is simple and rapid, and demonstrates a separation technique applicable to other acidic and basic drugs. It requires only extraction of the drug with methanol--water--acetic acid (66 + 33 + 1) and separation of insoluble material by filtration before HPLC. Labetalol, is chromatographically separated from soluble feed components by means of a microBondapak C18 column and methanol--water--acetic acid (66 + 33 + 1) mobile phase, 0.005M with respect to sodium dioctylsulfosuccinate paired-ion reagent. Average recovery is 98.7% with a relative standard deviation of +/- 2.3% for the equipment described.

Facile Preparation of Nanostructured, Superhydrophobic Filter Paper for Efficient Water/Oil Separation

PubMed Central

Wang, Jianhua; Wong, Jessica X. H.; Kwok, Honoria; Li, Xiaochun; Yu, Hua-Zhong

2016-01-01

In this paper, we present a facile and cost-effective method to obtain superhydrophobic filter paper and demonstrate its application for efficient water/oil separation. By coupling structurally distinct organosilane precursors (e.g., octadecyltrichlorosilane and methyltrichlorosilane) to paper fibers under controlled reaction conditions, we have formulated a simple, inexpensive, and efficient protocol to achieve a desirable superhydrophobic and superoleophilic surface on conventional filter paper. The silanized superhydrophobic filter paper showed nanostructured morphology and demonstrated great separation efficiency (up to 99.4%) for water/oil mixtures. The modified filter paper is stable in both aqueous solutions and organic solvents, and can be reused multiple times. The present study shows that our newly developed binary silanization is a promising method of modifying cellulose-based materials for practical applications, in particular the treatment of industrial waste water and ecosystem recovery. PMID:26982055

Development and evaluation of polyvinyl-alcohol blend polymer films as battery separators

NASA Technical Reports Server (NTRS)

Manzo, M. A.

1982-01-01

Several dialdehydes and epoxies were evaluated for their suitability as cross-linkers. Optium concentrations of several cross-linking reagents were determined. A two-step method of cross-linking, which involves treatment of the film in an acid or acid periodate bath, was investigated and dropped in favor of a one-step method in which the acid catalyst, which initiates cross-linking, is added to the PVA - cross-linker solution before casting. The cross-linking was thus achieved during the drying step. This one-step method was much more adaptable to commercial processing. Cross-linked films were characterized as alkaline battery separators. Films were prepared in the lab and tested in cells in order to evaluate the effect of film composition and a number of processing parameters on cell performance. These tests were conducted in order to provide a broader data base from which to select optimum processing parameters. Results of the separator screening tests and the cell tests are discussed.

Comparison of hydrochemical tracers to estimate source contributions to peak flow in a small, forested, headwater catchment

USGS Publications Warehouse

Rice, Karen C.; Hornberger, George M.

1998-01-01

Three-component (throughfall, soil water, groundwater) hydrograph separations at peak flow were performed on 10 storms over a 2-year period in a small forested catchment in north-central Maryland using an iterative and an exact solution. Seven pairs of tracers (deuterium and oxygen 18, deuterium and chloride, deuterium and sodium, deuterium and silica, chloride and silica, chloride and sodium, and sodium and silica) were used for three-component hydrograph separation for each storm at peak flow to determine whether or not the assumptions of hydrograph separation routinely can be met, to assess the adequacy of some commonly used tracers, to identify patterns in hydrograph-separation results, and to develop conceptual models for the patterns observed. Results of the three-component separations were not always physically meaningful, suggesting that assumptions of hydrograph separation had been violated. Uncertainties in solutions to equations for hydrograph separations were large, partly as a result of violations of assumptions used in deriving the separation equations and partly as a result of improper identification of chemical compositions of end-members. Results of three-component separations using commonly used tracers were widely variable. Consistent patterns in the amount of subsurface water contributing to peak flow (45-100%) were observed, no matter which separation method or combination of tracers was used. A general conceptual model for the sequence of contributions from the three end-members could be developed for 9 of the 10 storms. Overall results indicated that hydrochemical and hydrometric measurements need to be coupled in order to perform meaningful hydrograph separations.

Model of separation performance of bilinear gradients in scanning format counter-flow gradient electrofocusing techniques.

PubMed

Shameli, Seyed Mostafa; Glawdel, Tomasz; Ren, Carolyn L

2015-03-01

Counter-flow gradient electrofocusing allows the simultaneous concentration and separation of analytes by generating a gradient in the total velocity of each analyte that is the sum of its electrophoretic velocity and the bulk counter-flow velocity. In the scanning format, the bulk counter-flow velocity is varying with time so that a number of analytes with large differences in electrophoretic mobility can be sequentially focused and passed by a single detection point. Studies have shown that nonlinear (such as a bilinear) velocity gradients along the separation channel can improve both peak capacity and separation resolution simultaneously, which cannot be realized by using a single linear gradient. Developing an effective separation system based on the scanning counter-flow nonlinear gradient electrofocusing technique usually requires extensive experimental and numerical efforts, which can be reduced significantly with the help of analytical models for design optimization and guiding experimental studies. Therefore, this study focuses on developing an analytical model to evaluate the separation performance of scanning counter-flow bilinear gradient electrofocusing methods. In particular, this model allows a bilinear gradient and a scanning rate to be optimized for the desired separation performance. The results based on this model indicate that any bilinear gradient provides a higher separation resolution (up to 100%) compared to the linear case. This model is validated by numerical studies. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Microprobes aluminosilicate ceramic membranes

DOEpatents

Anderson, Marc A.; Sheng, Guangyao

1993-01-01

Methods have been developed to make mixed alumina-silicate and aluminosilicate particulate microporous ceramic membranes. One method involves the making of separate alumina and silica sols which are then mixed. Another method involves the creation of a combined sol with aluminosilicate particles. The resulting combined alumina and silica membranes have high surface area, a very small pore size, and a very good temperature stability.

Analytical method development for the determination of emerging contaminants in water using supercritical-fluid chromatography coupled with diode-array detection.

PubMed

Del Carmen Salvatierra-Stamp, Vilma; Ceballos-Magaña, Silvia G; Gonzalez, Jorge; Ibarra-Galván, Valentin; Muñiz-Valencia, Roberto

2015-05-01

An analytical method using supercritical-fluid chromatography coupled with diode-array detection for the determination of seven emerging contaminants-two pharmaceuticals (carbamazepine and glyburide), three endocrine disruptors (17α-ethinyl estradiol, bisphenol A, and 17β-estradiol), one bactericide (triclosan), and one pesticide (diuron)-was developed and validated. These contaminants were chosen because of their frequency of use and their toxic effects on both humans and the environment. The optimized chromatographic separation on a Viridis BEH 2-EP column achieved baseline resolution for all compounds in less than 10 min. This separation was applied to environmental water samples after sample preparation. The optimized sample treatment involved a preconcentration step by means of solid-phase extraction using C18-OH cartridges. The proposed method was validated, finding recoveries higher than 94 % and limits of detection and limits of quantification in the range of 0.10-1.59 μg L(-1) and 0.31-4.83 μg L(-1), respectively. Method validation established the proposed method to be selective, linear, accurate, and precise. Finally, the method was successfully applied to environmental water samples.

Separation and determination of synthetic impurities of difloxacin by reversed-phase high-performance liquid chromatography.

PubMed

Rao, R Nageswara; Nagaraju, V

2004-11-19

A simple and rapid reversed-phase high-performance liquid chromatographic method for separation and determination of process-related impurities of difloxacin (DFL) was developed. The separation was achieved on a reversed-phase C(18) column using methanol-water-acetic acid (78:21.9:0.1, v/v/v) as a mobile solvent at a flow rate of 1.0 ml/min at 28 degrees C using UV detection at 230 nm. It was linear over a range of 0.03 x 10(-6) to 1.60 x 10(-6)g for process related impurities and 0.05 x 10(-6) to 2.40 x 10(-6)g for difloxacin. The detection limits were 0.009 x 10(-6) to 0.024 x 10(-6)g for all the compounds examined. The recoveries were found to be in the range of 97.6-102.0% for impurities as well as difloxacin. The precision and robustness of the method were evaluated. It was used for not only quality assurance, but also monitoring the synthetic reactions involved in the process development work of difloxacin. The method was found to be specific, precise and reliable for the determination of unreacted levels of raw materials, intermediates in the reaction mixtures and the finished products of difloxacin.

Interrogation of an autofluorescence-based method for protein fingerprinting.

PubMed

Siddaramaiah, Manjunath; Rao, Bola Sadashiva S; Joshi, Manjunath B; Datta, Anirbit; Sandya, S; Vishnumurthy, Vasudha; Chandra, Subhash; Nayak, Subramanya G; Satyamoorthy, Kapaettu; Mahato, Krishna K

2018-03-14

In the present study, we have designed a laser-induced fluorescence (LIF) based instrumentation and developed a sensitive methodology for the effective separation, visualization, identification and analysis of proteins on a single platform. In this method, intrinsic fluorescence spectra of proteins were detected after separation on 1 or 2 dimensional Sodium Dodecyl Sulfate-Tris(2-carboxyethyl)phosphine (SDS-TCEP) polyacrylamide gel electrophoresis (PAGE) and the data were analyzed. The MATLAB assisted software was designed for the development of PAGE fingerprint for the visualization of protein after 1- and 2-dimensional protein separation. These provided objective parameters of intrinsic fluorescence intensity, emission peak, molecular weight and isoelectric point using a single platform. Further, the current architecture could differentiate the overlapping proteins in the PAGE gels which otherwise were not identifiable by conventional staining, imaging and tagging methods. Categorization of the proteins based on the presence or absence of tyrosine or tryptophan residues and assigning the corresponding emission peaks (309-356 nm) with pseudo colors allowed the detection of proportion of proteins within the given spectrum. The present methodology doesn't use stains or tags, hence amenable to couple with mass spectroscopic measurements. This technique may have relevance in the field of proteomics that is used for innumerable applications. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Derivatization of organophosphorus nerve agent degradation products for gas chromatography with ICPMS and TOF-MS detection.

PubMed

Richardson, Douglas D; Caruso, Joseph A

2007-06-01

Separation and detection of seven V-type (venomous) and G-type (German) organophosphorus nerve agent degradation products by gas chromatography with inductively coupled plasma mass spectrometry (GC-ICPMS) is described. The nonvolatile alkyl phosphonic acid degradation products of interest included ethyl methylphosphonic acid (EMPA, VX acid), isopropyl methylphosphonic acid (IMPA, GB acid), ethyl hydrogen dimethylamidophosphate sodium salt (EDPA, GA acid), isobutyl hydrogen methylphosphonate (IBMPA, RVX acid), as well as pinacolyl methylphosphonic acid (PMPA), methylphosphonic acid (MPA), and cyclohexyl methylphosphonic acid (CMPA, GF acid). N-(tert-Butyldimethylsilyl)-N-methyltrifluroacetamide with 1% TBDMSCl was utilized to form the volatile TBDMS derivatives of the nerve agent degradation products for separation by GC. Exact mass confirmation of the formation of six of the TBDMS derivatives was obtained by GC-time of flight mass spectrometry (TOF-MS). The method developed here allowed for the separation and detection of all seven TBDMS derivatives as well as phosphate in less than ten minutes. Detection limits for the developed method were less than 5 pg with retention times and peak area precisions of less than 0.01 and 6%, respectively. This method was successfully applied to river water and soil matrices. To date this is the first work describing the analysis of chemical warfare agent (CWA) degradation products by GC-ICPMS.

Spatial weighting approach in numerical method for disaggregation of MDGs indicators

NASA Astrophysics Data System (ADS)

Permai, S. D.; Mukhaiyar, U.; Satyaning PP, N. L. P.; Soleh, M.; Aini, Q.

2018-03-01

Disaggregation use to separate and classify the data based on certain characteristics or on administrative level. Disaggregated data is very important because some indicators not measured on all characteristics. Detailed disaggregation for development indicators is important to ensure that everyone benefits from development and support better development-related policymaking. This paper aims to explore different methods to disaggregate national employment-to-population ratio indicator to province- and city-level. Numerical approach applied to overcome the problem of disaggregation unavailability by constructing several spatial weight matrices based on the neighbourhood, Euclidean distance and correlation. These methods can potentially be used and further developed to disaggregate development indicators into lower spatial level even by several demographic characteristics.

Method Development for Pesticide Residue Analysis in Farmland Soil using High Perfomance Liquid Chromatography

NASA Astrophysics Data System (ADS)

Theresia Djue Tea, Marselina; Sabarudin, Akhmad; Sulistyarti, Hermin

2018-01-01

A method for the determination of diazinon and chlorantraniliprole in soil samples has been developed. The analyte was extracted with acetonitrile from farmland soil sample. Determination and quantification of diazinon and chlorantraniliprole were perfomed by high perfomance liquid chromatography (HPLC) with an UV detector. Several parameters of HPLC method were optimized with respect to sensitivity, high resolution of separation, and accurate determination of diazinon and chlorantraniliprole. Optimum conditions for the separation of two pesticides were eluent composition of acetonitrile:water ratio of 60:40, 0.4 mL/min of flow rate, and 220 nm of wavelength. Under the optimum conditions, diazinon linearity was in the range from 1-25 ppm with R2 of 0.9976, 1.19 mgL-1 LOD, and 3.98 mgL-1 LOQ; while the linearity of chlorantraniliprole was in the range from 0.2-5 mgL-1 with R2 of 0.9972, 0.39 mgL-1 LOD, and 1.29 mgL-1 LOQ. When the method was applied to the soil sample, both pesticides showed acceptable recoveries for real sample of more than 85%: thus, the developed method meets the validation requirement. Under this developed method, the concentrations of both pesticides in the soil samples were below the LOD and LOQ (0.577 mgL-1 for diazinon and 0.007 mgL-1 for chlorantraniliprole). Therefore, it can be concluded that the soil samples used in this study have neither diazinon nor chlorantraniliprole.

Cu2+-imprinted cross-linked chitosan resin as micro-column packing materials for online chemiluminescence determination of trace copper.

PubMed

Nie, Feng; Hao, Liang; Gao, Mei; Wu, Yingchun; Li, Xinsheng; Yu, Sha

2011-01-01

The Cu(2+)-imprinted cross-linked chitosan resin was synthesized and the binding characteristic of the resin to Cu(2+) was evaluated. The prepared resin was packed into a micro-glass column and used as micro-separating column. The micro-separating column was connected into the chemiluminescence flow system and placed in front of the window of the photomultiplier tube. Based on the luminol-hydrogen peroxide chemiluminescence system, a flow injection online chemiluminescence method for determination of trace copper was developed and trace Cu(2+) in complex samples was successfully determined. The proposed method improved the shortcomings of chemiluminescence method's poor selectivity. Copyright © 2010 John Wiley & Sons, Ltd.

[Determination of sennosides and degraded products in the process of sennoside metabolism by HPLC].

PubMed

Sun, Yan; Li, Xuetuo; Yu, Xingju

2004-01-01

A method for the separation and determination of sennosides A and B and the main composition (sennidins A and B) in degraded products of sennosides by linear gradient high performance liquid chromatography has been developed. Separation conditions were as follows: column, a Spherisorb C18 column (250 mm x 4.6 mm i.d., 10 microm); column temperature, 40 degrees C; detection wavelength, 360 nm; mobile phase A, 1.25% acetic acid aqueous solution; mobile phase B, methanol; linear gradient, 100% A --> (20 min) 100% B. The method is effective, quick, accurate and reproducible. The satisfactory results show that this new method has certain practical values as an approach of real-time analysis in the process of sennoside metabolism.

Separating inverse spin Hall voltage and spin rectification voltage by inverting spin injection direction

NASA Astrophysics Data System (ADS)

Zhang, Wenxu; Peng, Bin; Han, Fangbin; Wang, Qiuru; Soh, Wee Tee; Ong, Chong Kim; Zhang, Wanli

2016-03-01

We develop a method for universally resolving the important issue of separating the inverse spin Hall effect (ISHE) from the spin rectification effect (SRE) signal. This method is based on the consideration that the two effects depend on the spin injection direction: The ISHE is an odd function of the spin injection direction while the SRE is independent on it. Thus, the inversion of the spin injection direction changes the ISHE voltage signal, while the SRE voltage remains. It applies generally to analyzing the different voltage contributions without fitting them to special line shapes. This fast and simple method can be used in a wide frequency range and has the flexibility of sample preparation.

Resource Constrained Planning of Multiple Projects with Separable Activities

NASA Astrophysics Data System (ADS)

Fujii, Susumu; Morita, Hiroshi; Kanawa, Takuya

In this study we consider a resource constrained planning problem of multiple projects with separable activities. This problem provides a plan to process the activities considering a resource availability with time window. We propose a solution algorithm based on the branch and bound method to obtain the optimal solution minimizing the completion time of all projects. We develop three methods for improvement of computational efficiency, that is, to obtain initial solution with minimum slack time rule, to estimate lower bound considering both time and resource constraints and to introduce an equivalence relation for bounding operation. The effectiveness of the proposed methods is demonstrated by numerical examples. Especially as the number of planning projects increases, the average computational time and the number of searched nodes are reduced.

Analysis and Modeling of Boundary Layer Separation Method (BLSM).

PubMed

Pethő, Dóra; Horváth, Géza; Liszi, János; Tóth, Imre; Paor, Dávid

2010-09-01

Nowadays rules of environmental protection strictly regulate pollution material emission into environment. To keep the environmental protection laws recycling is one of the useful methods of waste material treatment. We have developed a new method for the treatment of industrial waste water and named it boundary layer separation method (BLSM). We apply the phenomena that ions can be enriched in the boundary layer of the electrically charged electrode surface compared to the bulk liquid phase. The main point of the method is that the boundary layer at correctly chosen movement velocity can be taken out of the waste water without being damaged, and the ion-enriched boundary layer can be recycled. Electrosorption is a surface phenomenon. It can be used with high efficiency in case of large electrochemically active surface of electrodes. During our research work two high surface area nickel electrodes have been prepared. The value of electrochemically active surface area of electrodes has been estimated. The existence of diffusion part of the double layer has been experimentally approved. The electrical double layer capacity has been determined. Ion transport by boundary layer separation has been introduced. Finally we have tried to estimate the relative significance of physical adsorption and electrosorption.

Isolation of >1 nm Diameter Single-Wall Carbon Nanotube Species Using Aqueous Two-Phase Extraction.

PubMed

Fagan, Jeffrey A; Hároz, Erik H; Ihly, Rachelle; Gui, Hui; Blackburn, Jeffrey L; Simpson, Jeffrey R; Lam, Stephanie; Hight Walker, Angela R; Doorn, Stephen K; Zheng, Ming

2015-05-26

In this contribution we demonstrate the effective separation of single-wall carbon nanotube (SWCNT) species with diameters larger than 1 nm through multistage aqueous two-phase extraction (ATPE), including isolation at the near-monochiral species level up to at least the diameter range of SWCNTs synthesized by electric arc synthesis (1.3-1.6 nm). We also demonstrate that refined species are readily obtained from both the metallic and semiconducting subpopulations of SWCNTs and that this methodology is effective for multiple SWCNT raw materials. Using these data, we report an empirical function for the necessary surfactant concentrations in the ATPE method for separating different SWCNTs into either the lower or upper phase as a function of SWCNT diameter. This empirical correlation enables predictive separation design and identifies a subset of SWCNTs that behave unusually as compared to other species. These results not only dramatically increase the range of SWCNT diameters to which species selective separation can be achieved but also demonstrate that aqueous two-phase separations can be designed across experimentally accessible ranges of surfactant concentrations to controllably separate SWCNT populations of very small (∼0.62 nm) to very large diameters (>1.7 nm). Together, the results reported here indicate that total separation of all SWCNT species is likely feasible by the ATPE method, especially given future development of multistage automated extraction techniques.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kojima, S.; Yokosawa, M.; Matsuyama, M.

To study the practical application of a tritium separation process using Self-Developing Gas Chromatography (SDGC) using a Pd-Pt alloy, intermediate scale-up experiments (22 mm ID x 2 m length column) and the development of a computational simulation method have been conducted. In addition, intermediate scale production of Pd-Pt powder has been developed for the scale-up experiments.The following results were obtained: (1) a 50-fold scale-up from 3 mm to 22 mm causes no significant impact on the SDGC process; (2) the Pd-Pt alloy powder is applicable to a large size SDGC process; and (3) the simulation enables preparation of a conceptualmore » design of a SDGC process for tritium separation.« less

Metal-Organic Frameworks for Separation.

PubMed

Zhao, Xiang; Wang, Yanxiang; Li, Dong-Sheng; Bu, Xianhui; Feng, Pingyun

2018-03-27

Separation is an important industrial step with critical roles in the chemical, petrochemical, pharmaceutical, and nuclear industries, as well as in many other fields. Although much progress has been made, the development of better separation technologies, especially through the discovery of high-performance separation materials, continues to attract increasing interest due to concerns over factors such as efficiency, health and environmental impacts, and the cost of existing methods. Metal-organic frameworks (MOFs), a rapidly expanding family of crystalline porous materials, have shown great promise to address various separation challenges due to their well-defined pore size and unprecedented tunability in both composition and pore geometry. In the past decade, extensive research is performed on applications of MOF materials, including separation and capture of many gases and vapors, and liquid-phase separation involving both liquid mixtures and solutions. MOFs also bring new opportunities in enantioselective separation and are amenable to morphological control such as fabrication of membranes for enhanced separation outcomes. Here, some of the latest progress in the applications of MOFs for several key separation issues, with emphasis on newly synthesized MOF materials and the impact of their compositional and structural features on separation properties, are reviewed and highlighted. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Recent developments on field gas extraction and sample preparation methods for radiokrypton dating of groundwater

NASA Astrophysics Data System (ADS)

Yokochi, Reika

2016-09-01

Current and foreseen population growths will lead to an increased demand in freshwater, large quantities of which is stored as groundwater. The ventilation age is crucial to the assessment of groundwater resources, complementing the hydrological model approach based on hydrogeological parameters. Ultra-trace radioactive isotopes of Kr (81 Kr and 85 Kr) possess the ideal physical and chemical properties for groundwater dating. The recent advent of atom trap trace analyses (ATTA) has enabled determination of ultra-trace noble gas radioisotope abundances using 5-10 μ L of pure Kr. Anticipated developments will enable ATTA to analyze radiokrypton isotope abundances at high sample throughput, which necessitates simple and efficient sample preparation techniques that are adaptable to various sample chemistries. Recent developments of field gas extraction devices and simple and rapid Kr separation method at the University of Chicago are presented herein. Two field gas extraction devices optimized for different sampling conditions were recently designed and constructed, aiming at operational simplicity and portability. A newly developed Kr purification system enriches Kr by flowing a sample gas through a moderately cooled (138 K) activated charcoal column, followed by a gentle fractionating desorption. This simple process uses a single adsorbent and separates 99% of the bulk atmospheric gases from Kr without significant loss. The subsequent two stages of gas chromatographic separation and a hot Ti sponge getter further purify the Kr-enriched gas. Abundant CH4 necessitates multiple passages through one of the gas chromatographic separation columns. The presented Kr separation system has a demonstrated capability of extracting Kr with > 90% yield and 99% purity within 75 min from 1.2 to 26.8 L STP of atmospheric air with various concentrations of CH4. The apparatuses have successfully been deployed for sampling in the field and purification of groundwater samples.

Application and recovery of ionic liquids in the preparative separation of four flavonoids from Rhodiola rosea by on-line three-dimensional liquid chromatography.

PubMed

Ma, Shufeng; Hu, Liming; Ma, Chaoyang; Lv, Wenping; Wang, Hongxin

2014-09-01

A novel on-line three-dimensional liquid chromatography method was developed to separate four main flavonoids from Rhodiola rosea. Ethyl acetate/0.5 mol/L ionic liquid 1-butyl-3-methylimidazolium chloride aqueous solution was selected as the solvent system. In the first-dimension separation, the target flavonoids were entrapped and subsequently desorbed into the second-dimension high-speed countercurrent chromatographic column for separation. In the third-dimension chromatography, the residual ionic liquid in the four separated flavonoids was removed and the used ionic liquid was recovered. As a result, 35.1 mg of compound 1, 20.4 mg of compound 2, 8.5 mg of compound 3, and 10.6 mg of compound 4 were obtained from 1.53 g R. rosea extract. They were identified as rhodiosin, rhodionin, herbacetin, and kaempferol, respectively. The recovery of ionic liquid reached 99.1% of the initial amount. The results showed that this method is a powerful technology for the separation of R. rosea flavonoids and that the ionic-liquid-based solvent system has advantages over traditional solvent systems in renewable and environmentally friendly properties. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Practices, Concerns, and Willingness to Participate in Solid Waste Management in Two Urban Slums in Central Uganda

PubMed Central

Ndejjo, Rawlance; Musoke, David; Musinguzi, Geofrey; Halage, Abdullah Ali; Carpenter, David O.; Ssempebwa, John C.

2016-01-01

Poor solid waste management is among the major challenges facing urban slums in developing countries including Uganda. Understanding community concerns and willingness towards involvement in solid waste management improvement initiatives is critical for informing interventions in slums. Methods. We used a cross-sectional study to collect quantitative data from 435 residents in two urban slums in central Uganda. A semistructured questionnaire was used which assessed waste collection practices, separation and disposal methods, concerns regarding solid wastes, and willingness to participate in waste separation and composting. Data was analysed using STATA 12. Results. Food remains (38%) and plastics (37%) formed the biggest proportion of wastes generated in households. Most households (35.9%) disposed of general wastes by open dumping while 27% disposed of plastics by burning. Only 8.8% of households conducted composting while 55% carried out separation for some decomposable wastes. Separation was carried out for only banana peelings and leftover foods for feeding animals. Respondents expressed high willingness to separate (76.6%) and compost (54.9%) solid wastes. Conclusion. Practices in waste disposal and separation were poor despite high willingness to participate in initiatives to improve waste management, highlighting a need for authorities to engage residents of slums to improve their practices. PMID:27066081

Module for phosphorus separation and recycling from liquid manures

USDA-ARS?s Scientific Manuscript database

A method has been developed to extract and concentrate soluble phosphates from livestock wastewater. The research was conducted over a 10-year period and went from initial bench studies and discovery, to pilot module development, to full-scale demonstrations of the phosphorus (P) module in swine fa...

Development and Validation of a Prototype Vacuum Sensing Unit for the DD2011 Chairside Amalgam Separators

DTIC Science & Technology

2015-10-30

pressure values onto the SD card. The addition of free and open-source Arduino libraries allowed for the seamless integration of the shield into the...alert the user when replacing the separator is necessary. Methods: A sensor was built to measure and record differential pressure values within the...from the transducers during simulated blockages were transformed into pressure values using linear regression equations from the calibration data

Physics-Based Computational Algorithm for the Multi-Fluid Plasma Model

DTIC Science & Technology

2014-06-30

applying it to study laser - 20 Physics-Based Multi-Fluid Plasma Algorithm Shumlak Figure 6: Blended finite element method applied to the species...separation problem in capsule implosions. Number densities and electric field are shown after the laser drive has compressed the multi-fluid plasma and...6 after the laser drive has started the compression. A separation clearly develops. The solution is found using an explicit advance (CFL=1) for the

Accelerator Production and Separations for High Specific Activity Rhenium-186

DOE Office of Scientific and Technical Information (OSTI.GOV)

Jurisson, Silvia S.; Wilbur, D. Scott

2016-04-01

Tungsten and osmium targets were evaluated for the production of high specific activity rhenium-186. Rhenium-186 has potential applications in radiotherapy for the treatment of a variety of diseases, including targeting with monoclonal antibodies and peptides. Methods were evaluated using tungsten metal, tungsten dioxide, tungsten disulfide and osmium disulfide. Separation of the rhenium-186 produced and recycling of the enriched tungsten-186 and osmium-189 enriched targets were developed.

Real-time modulated nanoparticle separation with an ultra-large dynamic range.

PubMed

Zeming, Kerwin Kwek; Thakor, Nitish V; Zhang, Yong; Chen, Chia-Hung

2016-01-07

Nanoparticles exhibit size-dependent properties which make size-selective purification of proteins, DNA or synthetic nanoparticles essential for bio-analytics, clinical medicine, nano-plasmonics and nano-material sciences. Current purification methods of centrifugation, column chromatography and continuous-flow techniques suffer from particle aggregation, multi-stage process, complex setups and necessary nanofabrication. These increase process costs and time, reduce efficiency and limit dynamic range. Here, we achieve an unprecedented real-time nanoparticle separation (51-1500 nm) using a large-pore (2 μm) deterministic lateral displacement (DLD) device. No external force fields or nanofabrication are required. Instead, we investigated innate long-range electrostatic influences on nanoparticles within a fluid medium at different NaCl ionic concentrations. In this study we account for the electrostatic forces beyond Debye length and showed that they cannot be assumed as negligible especially for precise nanoparticle separation methods such as DLD. Our findings have enabled us to develop a model to simultaneously quantify and modulate the electrostatic force interactions between nanoparticle and micropore. By simply controlling buffer solutions, we achieve dynamic nanoparticle size separation on a single device with a rapid response time (<20 s) and an enlarged dynamic range (>1200%), outperforming standard benchtop centrifuge systems. This novel method and model combines device simplicity, isolation precision and dynamic flexibility, opening opportunities for high-throughput applications in nano-separation for industrial and biological applications.

High-temperature LC-MS/MS of permethylated glycans derived from glycoproteins.

PubMed

Zhou, Shiyue; Hu, Yunli; Mechref, Yehia

2016-06-01

Various glycomic analysis methods have been developed due to the essential roles of glycans in biological processes as well as the potential application of glycomics in biomarker discovery in many diseases. Permethylation is currently considered to be one of the most common derivatization methods in MS-based glycomic analysis. Permethylation not only improves ionization efficiency and stability of sialylated glycans in positive mode but also allows for enhanced separation performance on reversed-phase liquid chromatography (RPLC). Recently, RPLC-MS analysis of permethylated glycans exhibited excellent performance in sensitivity and reproducibility and became a widely-applied comprehensive strategy in glycomics. However, separating permethylated glycans by RPLC always suffers from peak broadening for high-molecular-weight branched glycans, which probably due to the low exchange rate between the stationary phase and mobile phase limited by intermolecular interactions of the methyl groups associated with the branching of the glycan structures. In this study, we employed high separation temperature conditions for RPLC of permethylated glycans, thus achieving enhanced peak capacity, improving peak shape, and enhancing separation efficiency. Additionally, partial isomeric separation were observed in RPLC of permethylated glycans at high-temperature. Mathematical processing of the correlation between retention time and molecular weight also revealed the advantage of high-temperature LC method for both manual and automatic glycan identification. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ion chromatography with the indirect ultraviolet detection of alkali metal ions and ammonium using imidazolium ionic liquid as ultraviolet absorption reagent and eluent.

PubMed

Liu, Yong-Qiang; Yu, Hong

2016-08-01

Indirect ultraviolet detection was conducted in ultraviolet-absorption-agent-added mobile phase to complete the detection of the absence of ultraviolet absorption functional group in analytes. Compared with precolumn derivatization or postcolumn derivatization, this method can be widely used, has the advantages of simple operation and good linear relationship. Chromatographic separation of Li(+) , Na(+) , K(+) , and NH4 (+) was performed on a carboxylic acid base cation exchange column using imidazolium ionic liquid/acid/organic solvent as the mobile phase, in which imidazolium ionic liquids acted as ultraviolet absorption reagent and eluting agent. The retention behaviors of four kinds of cations are discussed, and the mechanism of separation and detection are described. The main factors influencing the separation and detection were the background ultraviolet absorption reagent and the concentration of hydrogen ion in the ion chromatography-indirect ultraviolet detection. The successful separation and detection of Li(+) , Na(+) , K(+) , and NH4 (+) within 13 min was achieved using the selected chromatographic conditions, and the detection limits (S/N = 3) were 0.02, 0.11, 0.30, and 0.06 mg/L, respectively. A new separation and analysis method of alkali metal ions and ammonium by ion chromatography with indirect ultraviolet detection method was developed, and the application range of ionic liquid was expanded. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of some phenolic compounds in red wine by RP-HPLC: method development and validation.

PubMed

Burin, Vívian Maria; Arcari, Stefany Grützmann; Costa, Léa Luzia Freitas; Bordignon-Luiz, Marilde T

2011-09-01

A methodology employing reversed-phase high-performance liquid chromatography (RP-HPLC) was developed and validated for simultaneous determination of five phenolic compounds in red wine. The chromatographic separation was carried out in a C(18) column with water acidify with acetic acid (pH 2.6) (solvent A) and 20% solvent A and 80% acetonitrile (solvent B) as the mobile phase. The validation parameters included: selectivity, linearity, range, limits of detection and quantitation, precision and accuracy, using an internal standard. All calibration curves were linear (R(2) > 0.999) within the range, and good precision (RSD < 2.6%) and recovery (80-120%) was obtained for all compounds. This method was applied to quantify phenolics in red wine samples from Santa Catarina State, Brazil, and good separation peaks for phenolic compounds in these wines were observed.

Acetanilide 4-hydroxylase and acetanilide 2-hydroxylase activity in hepatic microsomes from induced mice.

PubMed

Lewandowski, M; Chui, Y C; Levi, P; Hodgson, E

1991-02-01

A simple and sensitive method for the separation of 14C-labelled acetanilide, 4-hydroxyacetanilide, 3-hydroxyacetanilide and 2-hydroxyacetanilide was developed using thin-layer chromatography. This separation is the basis for the assay of acetanilide 4-hydroxylase and acetanilide 2-hydroxylase activity in liver microsomes from DBA2/N male mice that had been treated with phenobarbital, 3-methylcholanthrene, isosafrole or n-butylbenzodioxole. Microsomes were incubated with [14C]acetanilide and extracted with benzene and ethyl acetate. The extract was applied to silica gel plates and developed with a hexane/isopropanol/ammonium hydroxide/water solvent system. The radiolabelled phenolic metabolites and the parent compound were detected using a Berthold Automatic TLC Linear Analyzer. Although the 4-hydroxylated metabolite was the primary product detected, this method can be used to detect other phenolic metabolites.

Charge-based separation of particles and cells with similar sizes via the wall-induced electrical lift.

PubMed

Thomas, Cory; Lu, Xinyu; Todd, Andrew; Raval, Yash; Tzeng, Tzuen-Rong; Song, Yongxin; Wang, Junsheng; Li, Dongqing; Xuan, Xiangchun

2017-01-01

The separation of particles and cells in a uniform mixture has been extensively studied as a necessity in many chemical and biomedical engineering and research fields. This work demonstrates a continuous charge-based separation of fluorescent and plain spherical polystyrene particles with comparable sizes in a ψ-shaped microchannel via the wall-induced electrical lift. The effects of both the direct current electric field in the main-branch and the electric field ratio in between the inlet branches for sheath fluid and particle mixture are investigated on this electrokinetic particle separation. A Lagrangian tracking method based theoretical model is also developed to understand the particle transport in the microchannel and simulate the parametric effects on particle separation. Moreover, the demonstrated charge-based separation is applied to a mixture of yeast cells and polystyrene particles with similar sizes. Good separation efficiency and purity are achieved for both the cells and the particles. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Adaptable bioinspired special wetting surface for multifunctional oil/water separation

NASA Astrophysics Data System (ADS)

Kavalenka, Maryna N.; Vüllers, Felix; Kumberg, Jana; Zeiger, Claudia; Trouillet, Vanessa; Stein, Sebastian; Ava, Tanzila T.; Li, Chunyan; Worgull, Matthias; Hölscher, Hendrik

2017-01-01

Inspired by the multifunctionality of biological surfaces necessary for the survival of an organism in its specific environment, we developed an artificial special wetting nanofur surface which can be adapted to perform different functionalities necessary to efficiently separate oil and water for cleaning accidental oil spills or separating industrial oily wastewater. Initial superhydrophobic nanofur surface is fabricated using a hot pulling method, in which nano- and microhairs are drawn out of the polymer surface during separation from a heated sandblasted steel plate. By using a set of simple modification techniques, which include microperforation, plasma treatment and subsequent control of storage environment, we achieved selective separation of either water or oil, variable oil absorption and continuous gravity driven separation of oil/water mixtures by filtration. Furthermore, these functions can be performed using special wetting nanofur made from various thermoplastics, including biodegradable and recyclable polymers. Additionally, nanofur can be reused after washing it with organic solvents, thus, further helping to reduce the environmental impacts of oil/water separation processes.

Adaptable bioinspired special wetting surface for multifunctional oil/water separation

PubMed Central

Kavalenka, Maryna N.; Vüllers, Felix; Kumberg, Jana; Zeiger, Claudia; Trouillet, Vanessa; Stein, Sebastian; Ava, Tanzila T.; Li, Chunyan; Worgull, Matthias; Hölscher, Hendrik

2017-01-01

Inspired by the multifunctionality of biological surfaces necessary for the survival of an organism in its specific environment, we developed an artificial special wetting nanofur surface which can be adapted to perform different functionalities necessary to efficiently separate oil and water for cleaning accidental oil spills or separating industrial oily wastewater. Initial superhydrophobic nanofur surface is fabricated using a hot pulling method, in which nano- and microhairs are drawn out of the polymer surface during separation from a heated sandblasted steel plate. By using a set of simple modification techniques, which include microperforation, plasma treatment and subsequent control of storage environment, we achieved selective separation of either water or oil, variable oil absorption and continuous gravity driven separation of oil/water mixtures by filtration. Furthermore, these functions can be performed using special wetting nanofur made from various thermoplastics, including biodegradable and recyclable polymers. Additionally, nanofur can be reused after washing it with organic solvents, thus, further helping to reduce the environmental impacts of oil/water separation processes. PMID:28051163

Rapid filtration separation-based sample preparation method for Bacillus spores in powdery and environmental matrices.

PubMed

Isabel, Sandra; Boissinot, Maurice; Charlebois, Isabelle; Fauvel, Chantal M; Shi, Lu-E; Lévesque, Julie-Christine; Paquin, Amélie T; Bastien, Martine; Stewart, Gale; Leblanc, Eric; Sato, Sachiko; Bergeron, Michel G

2012-03-01

Authorities frequently need to analyze suspicious powders and other samples for biothreat agents in order to assess environmental safety. Numerous nucleic acid detection technologies have been developed to detect and identify biowarfare agents in a timely fashion. The extraction of microbial nucleic acids from a wide variety of powdery and environmental samples to obtain a quality level adequate for these technologies still remains a technical challenge. We aimed to develop a rapid and versatile method of separating bacteria from these samples and then extracting their microbial DNA. Bacillus atrophaeus subsp. globigii was used as a simulant of Bacillus anthracis. We studied the effects of a broad variety of powdery and environmental samples on PCR detection and the steps required to alleviate their interference. With a benchmark DNA extraction procedure, 17 of the 23 samples investigated interfered with bacterial lysis and/or PCR-based detection. Therefore, we developed the dual-filter method for applied recovery of microbial particles from environmental and powdery samples (DARE). The DARE procedure allows the separation of bacteria from contaminating matrices that interfere with PCR detection. This procedure required only 2 min, while the DNA extraction process lasted 7 min, for a total of <10 min. This sample preparation procedure allowed the recovery of cleaned bacterial spores and relieved detection interference caused by a wide variety of samples. Our procedure was easily completed in a laboratory facility and is amenable to field application and automation.

Rapid Filtration Separation-Based Sample Preparation Method for Bacillus Spores in Powdery and Environmental Matrices

PubMed Central

Isabel, Sandra; Boissinot, Maurice; Charlebois, Isabelle; Fauvel, Chantal M.; Shi, Lu-E; Lévesque, Julie-Christine; Paquin, Amélie T.; Bastien, Martine; Stewart, Gale; Leblanc, Éric; Sato, Sachiko

2012-01-01

Authorities frequently need to analyze suspicious powders and other samples for biothreat agents in order to assess environmental safety. Numerous nucleic acid detection technologies have been developed to detect and identify biowarfare agents in a timely fashion. The extraction of microbial nucleic acids from a wide variety of powdery and environmental samples to obtain a quality level adequate for these technologies still remains a technical challenge. We aimed to develop a rapid and versatile method of separating bacteria from these samples and then extracting their microbial DNA. Bacillus atrophaeus subsp. globigii was used as a simulant of Bacillus anthracis. We studied the effects of a broad variety of powdery and environmental samples on PCR detection and the steps required to alleviate their interference. With a benchmark DNA extraction procedure, 17 of the 23 samples investigated interfered with bacterial lysis and/or PCR-based detection. Therefore, we developed the dual-filter method for applied recovery of microbial particles from environmental and powdery samples (DARE). The DARE procedure allows the separation of bacteria from contaminating matrices that interfere with PCR detection. This procedure required only 2 min, while the DNA extraction process lasted 7 min, for a total of <10 min. This sample preparation procedure allowed the recovery of cleaned bacterial spores and relieved detection interference caused by a wide variety of samples. Our procedure was easily completed in a laboratory facility and is amenable to field application and automation. PMID:22210204

Model reduction method using variable-separation for stochastic saddle point problems

NASA Astrophysics Data System (ADS)

Jiang, Lijian; Li, Qiuqi

2018-02-01

In this paper, we consider a variable-separation (VS) method to solve the stochastic saddle point (SSP) problems. The VS method is applied to obtain the solution in tensor product structure for stochastic partial differential equations (SPDEs) in a mixed formulation. The aim of such a technique is to construct a reduced basis approximation of the solution of the SSP problems. The VS method attempts to get a low rank separated representation of the solution for SSP in a systematic enrichment manner. No iteration is performed at each enrichment step. In order to satisfy the inf-sup condition in the mixed formulation, we enrich the separated terms for the primal system variable at each enrichment step. For the SSP problems by regularization or penalty, we propose a more efficient variable-separation (VS) method, i.e., the variable-separation by penalty method. This can avoid further enrichment of the separated terms in the original mixed formulation. The computation of the variable-separation method decomposes into offline phase and online phase. Sparse low rank tensor approximation method is used to significantly improve the online computation efficiency when the number of separated terms is large. For the applications of SSP problems, we present three numerical examples to illustrate the performance of the proposed methods.

Three dimensional liquid chromatography coupling ion exchange chromatography/hydrophobic interaction chromatography/reverse phase chromatography for effective protein separation in top-down proteomics.

PubMed

Valeja, Santosh G; Xiu, Lichen; Gregorich, Zachery R; Guner, Huseyin; Jin, Song; Ge, Ying

2015-01-01

To address the complexity of the proteome in mass spectrometry (MS)-based top-down proteomics, multidimensional liquid chromatography (MDLC) strategies that can effectively separate proteins with high resolution and automation are highly desirable. Although various MDLC methods that can effectively separate peptides from protein digests exist, very few MDLC strategies, primarily consisting of 2DLC, are available for intact protein separation, which is insufficient to address the complexity of the proteome. We recently demonstrated that hydrophobic interaction chromatography (HIC) utilizing a MS-compatible salt can provide high resolution separation of intact proteins for top-down proteomics. Herein, we have developed a novel 3DLC strategy by coupling HIC with ion exchange chromatography (IEC) and reverse phase chromatography (RPC) for intact protein separation. We demonstrated that a 3D (IEC-HIC-RPC) approach greatly outperformed the conventional 2D IEC-RPC approach. For the same IEC fraction (out of 35 fractions) from a crude HEK 293 cell lysate, a total of 640 proteins were identified in the 3D approach (corresponding to 201 nonredundant proteins) as compared to 47 in the 2D approach, whereas simply prolonging the gradients in RPC in the 2D approach only led to minimal improvement in protein separation and identifications. Therefore, this novel 3DLC method has great potential for effective separation of intact proteins to achieve deep proteome coverage in top-down proteomics.

Detection of malondialdehyde in processed meat products without interference from the ingredients.

PubMed

Jung, Samooel; Nam, Ki Chang; Jo, Cheorun

2016-10-15

Our aim was to develop a method for accurate quantification of malondialdehyde (MDA) in meat products. MDA content of uncured ground pork (Control); ground pork cured with sodium nitrite (Nitrite); and ground pork cured with sodium nitrite, sodium chloride, sodium pyrophosphate, maltodextrin, and a sausage seasoning (Mix) was measured by the 2-thiobarbituric acid (TBA) assay with MDA extraction by trichloroacetic acid (method A) and two high-performance liquid chromatography (HPLC) methods: i) HPLC separation of the MDA-dinitrophenyl hydrazine adduct (method B) and ii) HPLC separation of MDA (method C) after MDA extraction with acetonitrile. Methods A and B could not quantify MDA accurately in groups Nitrite and Mix. Nevertheless, MDA in groups Control, Nitrite, and Mix was accurately quantified by method C with good recovery. Therefore, direct MDA quantification by HPLC after MDA extraction with acetonitrile (method C) is useful for accurate measurement of MDA content in processed meat products. Copyright © 2016 Elsevier Ltd. All rights reserved.

Colorimetric determination of alkaline phosphatase as indicator of mammalian feces in corn meal: collaborative study.

PubMed

Gerber, H

1986-01-01

In the official method for rodent filth in corn meal, filth and corn meal are separated in organic solvents, and particles are identified by the presence of hair and a mucous coating. The solvents are toxic, poor separation yields low recoveries, and fecal characteristics are rarely present on all fragments, especially on small particles. The official AOAC alkaline phosphatase test for mammalian feces, 44.181-44.184, has therefore been adapted to determine the presence of mammalian feces in corn meal. The enzyme cleaves phosphate radicals from a test indicator/substrate, phenolphthalein diphosphate. As free phenolphthalein accumulates, a pink-to-red color develops in the gelled test agar medium. In a collaborative study conducted to compare the proposed method with the official method for corn meal, 44.049, the proposed method yielded 45.5% higher recoveries than the official method. Repeatability and reproducibility for the official method were roughly 1.8 times more variable than for the proposed method. The method has been adopted official first action.

Development and Optimisation of an HPLC-DAD-ESI-Q-ToF Method for the Determination of Phenolic Acids and Derivatives

PubMed Central

Restivo, Annalaura; Degano, Ilaria; Ribechini, Erika; Colombini, Maria Perla

2014-01-01

A method for the HPLC-MS/MS analysis of phenols, including phenolic acids and naphtoquinones, using an amide-embedded phase column was developed and compared to the literature methods based on classical C18 stationary phase columns. RP-Amide is a recently developed polar embedded stationary phase, whose wetting properties mean that up to 100% water can be used as an eluent. The increased retention and selectivity for polar compounds and the possibility of working in 100% water conditions make this column particularly interesting for the HPLC analysis of phenolic acids and derivatives. In this study, the chromatographic separation was optimised on an HPLC-DAD, and was used to separate 13 standard phenolic acids and derivatives. The method was validated on an HPLC-ESI-Q-ToF. The acquisition was performed in negative polarity and MS/MS target mode. Ionisation conditions and acquisition parameters for the Q-ToF detector were investigated by working on collision energies and fragmentor potentials. The performance of the method was fully evaluated on standards. Moreover, several raw materials containing phenols were analysed: walnut, gall, wine, malbec grape, French oak, red henna and propolis. Our method allowed us to characterize the phenolic composition in a wide range of matrices and to highlight possible matrix effects. PMID:24551158

Fabrication of superhydrophilic and underwater superoleophobic metal mesh by laser treatment and its application

NASA Astrophysics Data System (ADS)

Yu, Peng; Lian, Zhongxu; Xu, Jinkai; Yu, Zhanjiang; Ren, Wanfei; Yu, Huadong

2018-04-01

In this paper, a lot of micron-sized sand granular structures were formed on the substrate of the stainless steel mesh (SSM) by laser treatment. The rough surface with sand granular structures showed superhydrophilic in air and superoleophobic under water. With its special wettability, the SSM by laser treatment could achieve the separation of the oil/water mixture, showing good durability and high separation efficiency, which was very useful in the practical application of large-scale oil/water separation facility for reducing the impacts of oil leaked on the environment. In addition, it showed that the laser-treated SSM had a very high separation rate. The development of the laser-treated SSM is a simple, environmental, economical and high-efficiency method, which provides a new approach to the production of high efficiency facilities for oil/water separation.

A general range-separated double-hybrid density-functional theory

NASA Astrophysics Data System (ADS)

Kalai, Cairedine; Toulouse, Julien

2018-04-01

A range-separated double-hybrid (RSDH) scheme which generalizes the usual range-separated hybrids and double hybrids is developed. This scheme consistently uses a two-parameter Coulomb-attenuating-method (CAM)-like decomposition of the electron-electron interaction for both exchange and correlation in order to combine Hartree-Fock exchange and second-order Møller-Plesset (MP2) correlation with a density functional. The RSDH scheme relies on an exact theory which is presented in some detail. Several semi-local approximations are developed for the short-range exchange-correlation density functional involved in this scheme. After finding optimal values for the two parameters of the CAM-like decomposition, the RSDH scheme is shown to have a relatively small basis dependence and to provide atomization energies, reaction barrier heights, and weak intermolecular interactions globally more accurate or comparable to range-separated MP2 or standard MP2. The RSDH scheme represents a new family of double hybrids with minimal empiricism which could be useful for general chemical applications.

Microchip Immunoaffinity Electrophoresis of Antibody-Thymidine Kinase 1 Complex

PubMed Central

Pagaduan, Jayson V.; Ramsden, Madison; O’Neill, Kim; Woolley, Adam T.

2015-01-01

Thymidine kinase-1 (TK1) is an important cancer biomarker whose serum levels are elevated in early cancer development. We developed a microchip electrophoresis immunoaffinity assay to measure recombinant purified TK1 (pTK1) using an antibody that binds to human TK1. We fabricated poly(methyl methacrylate) microfluidic devices to test the feasibility of detecting antibody (Ab)-pTK1 immune complexes as a step towards TK1 analysis in clinical serum samples. We were able to separate immune complexes from unbound antibodies using 0.5X phosphate buffer saline (pH 7.4) containing 0.01% Tween-20, with 1% w/v methylcellulose that acts as a dynamic surface coating and sieving matrix. Separation of the antibody and Ab-pTK1 complex was observed within a 5 mm effective separation length. This method of detecting pTK1 is easy to perform, requires only a 10 μL sample volume, and takes just 1 minute for separation. PMID:25486911

Native red electrophoresis--a new method suitable for separation of native proteins.

PubMed

Dráb, Tomáš; Kračmerová, Jana; Tichá, Ivana; Hanzlíková, Eva; Tichá, Marie; Ryšlavá, Helena; Doubnerová, Veronika; Maňásková-Postlerová, Pavla; Liberda, Jiří

2011-12-01

A new type of native electrophoresis was developed to separate and characterize proteins. In this modification of the native blue electrophoresis, the dye Ponceau Red S is used instead of Coomassie Brilliant Blue to impose uniform negative charge on proteins to enable their electrophoretic separation according to their relative molecular masses. As Ponceau Red S binds less tightly to proteins, in comparison with Coomassie Blue, it can be easily removed after the electrophoretic separation and a further investigation of protein properties is made possible (e.g. an enzyme detection or electroblotting). The tested proteins also kept their native properties (enzyme activity or aggregation state). Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Dynamic Sonographic Visualization of an Occult Posterior Lateral Meniscocapsular Separation: A Case Report.

PubMed

Schroeder, Allison; Musahl, Volker; Urbanek, Christopher; Onishi, Kentaro

2018-04-05

Meniscocapsular separation describes detachment of the meniscus from the knee joint capsule. Diagnosis is challenging with conventional examination and imaging methods. We report a case of an 18-year-old female softball catcher with unrevealing magnetic resonance imaging despite continued left knee locking and discomfort with deep squatting. Meniscocapsular separation was revealed only on dynamic sonographic exam, where knee flexion revealed a 3.1-mm gap that developed between the capsule and peripheral meniscus. Arthroscopy confirmed the sonographic findings, and repair resulted in complete resolution of symptoms. This case highlights the utility of dynamic diagnostic sonography in a rare case of posterior lateral meniscocapsular separation. Copyright © 2018 American Academy of Physical Medicine and Rehabilitation. Published by Elsevier Inc. All rights reserved.

Determination of fat- and water-soluble vitamins by supercritical fluid chromatography: A review.

PubMed

Tyśkiewicz, Katarzyna; Dębczak, Agnieszka; Gieysztor, Roman; Szymczak, Tomasz; Rój, Edward

2018-01-01

Vitamins are compounds that take part in all basic functions of an organism but also are subject of number of studies performed by different researchers. Two groups of vitamins are distinguished taking into consideration their solubility. Chromatography with supercritical CO 2 has found application in the determination, separation, and quantitative analyses of both fat- and water-soluble vitamins. The methods of vitamins separation have developed and improved throughout the years. Both groups of compounds were separated using supercritical fluid chromatography with different detection on different stationary phases. The main aim of this review is to provide an overview of the studies of vitamins separation that have been determined so far. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Injection by hydrostatic pressure in conjunction with electrokinetic force on a microfluidic chip.

PubMed

Gai, Hongwei; Yu, Linfen; Dai, Zhongpeng; Ma, Yinfa; Lin, Bingcheng

2004-06-01

A simple method was developed for injecting a sample on a cross-form microfluidic chip by means of hydrostatic pressure combined with electrokinetic forces. The hydrostatic pressure was generated simply by adjusting the liquid level in different reservoirs without any additional driven equipment such as a pump. Two dispensing strategies using a floating injection and a gated injection, coupled with hydrostatic pressure loading, were tested. The fluorescence observation verified the feasibility of hydrostatic pressure loading in the separation of a mixture of fluorescein sodium salt and fluorescein isothiocyanate. This method was proved to be effective in leading cells to a separation channel for single cell analysis.

Behavior of new complexes of tetrakis(4-methoxylphenyl)porphyrin with heavy rare earth elements in reversed-phase high performance liquid chromatography.

PubMed

Zhang, Jun-Feng; Wang, Hong; Hou, An-Xin; Wang, Chang-Fa; Zhang, Hua-Shan

2004-08-01

An HPLC method has been developed for the separation of new complexes of tetrakis(4-methoxylphenyl)porphyrin (TMOPP) with four heavy rare earth elements (RE = Y, Er, Tm, and Yb). The function of amine and acid in the mobile phase has been investigated and a reasonable explanation is presented. Successful separation of the RE-TMOPP-Cl complexes is accomplished in 10 min with a mobile phase consisting of methanol-water-acetic acid-triethanolamine. The detection limits (S/N= 3) for the four complexes are 0.01 microg/mL. This method is rapid, sensitive, and simple.

Automatic corn-soybean classification using Landsat MSS data. I - Near-harvest crop proportion estimation. II - Early season crop proportion estimation

NASA Technical Reports Server (NTRS)

Badhwar, G. D.

1984-01-01

The techniques used initially for the identification of cultivated crops from Landsat imagery depended greatly on the iterpretation of film products by a human analyst. This approach was not very effective and objective. Since 1978, new methods for crop identification are being developed. Badhwar et al. (1982) showed that multitemporal-multispectral data could be reduced to a simple feature space of alpha and beta and that these features would separate corn and soybean very well. However, there are disadvantages related to the use of alpha and beta parameters. The present investigation is concerned with a suitable method for extracting the required features. Attention is given to a profile model for crop discrimination, corn-soybean separation using profile parameters, and an automatic labeling (target recognition) method. The developed technique is extended to obtain a procedure which makes it possible to estimate the crop proportion of corn and soybean from Landsat data early in the growing season.

Grinding and cooking dry-mill germ to optimize aqueous enzymatic oil extraction

USDA-ARS?s Scientific Manuscript database

The many recent dry grind plants that convert corn to ethanol are potential sources of substantial amounts of corn oil. This report describes an aqueous enzymatic extraction (AEE) method to separate oil from dry-mill corn germ (DMG). The method is an extension of AEE previously developed for wet...

Magnetic anomalies in east Pacific using MAGSAT data

NASA Technical Reports Server (NTRS)

Harrison, C. G. A. (Principal Investigator)

1983-01-01

Methods for solving problems encountered in separating the core field from the crustal field are summarized as well as those methods developed for inverting total magnetic field data to obtain source functions for oceanic areas. Accounting for magnetization contrasts and the magnetization values measured in rocks of marine origin are also discussed.

Synthesis of amino-rich silica coated magnetic nanoparticles and their application in the capture of DNA for PCR

USDA-ARS?s Scientific Manuscript database

Magnetic separation has great advantages over traditional bioseparation methods and has become popular in the development of methods for the detection of bacterial pathogens, viruses, and transgenic crops. Functionalization of magnetic nanoparticles is a key factor in allowing efficient capture of t...

Determination of citrus limonoid glucosides by high performance liquid chromatography coupled to post-column reaction with Ehrlich’s Reagent

USDA-ARS?s Scientific Manuscript database

A method for the identification and quantification of citrus limonoid glucosides in juices based upon high performance liquid chromatography (HPLC) separation coupled to post-column reaction with Ehrlichs’s reagent has been developed. This method utilizes a phenyl stationary phase and an isocratic ...

Improving automated disturbance maps using snow-covered landsat time series stacks

Treesearch

Kirk M. Stueve; Ian W. Housman; Patrick L. Zimmerman; Mark D. Nelson; Jeremy Webb; Charles H. Perry; Robert A. Chastain; Dale D. Gormanson; Chengquan Huang; Sean P. Healey; Warren B. Cohen

2012-01-01

Snow-covered winter Landsat time series stacks are used to develop a nonforest mask to enhance automated disturbance maps produced by the Vegetation Change Tracker (VCT). This method exploits the enhanced spectral separability between forested and nonforested areas that occurs with sufficient snow cover. This method resulted in significant improvements in Vegetation...

Precolumn derivatization followed by liquid chromatographic separation and determination of tramiprosate in rat plasma by fluorescence detector: application to pharmacokinetics.

PubMed

Rao, R Nageswara; Maurya, Pawan K; Shinde, Dhananjay D; Khalid, Sara

2011-05-15

Alzheimer disease (AD) is characterized pathologically by extracellular amyloid deposits composed of amyloid β (Aβ) protein. A simple and rapid method using HPLC with fluorescence detector was developed and validated for determination of tramiprosate in rat plasma. Pre-column derivatization of the deproteinized rat plasma was carried out using o-phthaldialdehyde (OPA) as a fluorescent reagent in presence of 3-mercaptopropionic acid. The liquid chromatographic separation was achieved on a Kromasil C18 column using methanol:acetonitrile: 20 mM phosphate buffer pH 7.5 (8.0:17.5:74.5 v/v/v) as a mobile phase in an isocratic elution mode. The eluents were monitored by a fluorescence detector set at 330 and 450 nm of excitation and emission wavelength respectively. Vigabatrin was used as an internal standard. The method was linear within the range 30.0-1000.0 ng/mL. Design of experiments (DOE) was used to evaluate the robustness of the method. The developed method was applied to study the pharmacokinetics of tramiprosate in rats. Copyright © 2011. Published by Elsevier B.V.

Development of a novel molecular detection method for clustered regularly interspaced short palindromic repeats (CRISPRs) in Taylorella organisms.

PubMed

Hara, Yasushi; Nakajima, Takuya; Akamatsu, Marie; Yahiro, Motoki; Kagawa, Shizuko; Petry, Sandrine; Matsuda, Motoo; Moore, John E

2015-07-01

Contagious equine metritis is a bacterial infectious disease of horses caused by Taylorella equigenitalis, a Gram-negative eubacterium. The disease has been described in several continents, including Europe, North America and Asia. A novel molecular method was developed to detect clustered regularly interspaced short palindromic repeats (CRISPRs), which were separated by non-repetitive unique spacer regions (NRUSRs) of similar length, in the Taylorella equigenitalis EQ59 strain using a primer pair, f-/r-TeCRISPR-ladder, by PCR amplification. In total, 31 Taylorella isolates (17 T. equigenitalis and 14 Taylorella asinigenitalis) were examined. The T. equigenitalis isolates came from thoroughbred and cold-blooded horses from nine countries during 1980-1996, whilst the T. asinigenitalis isolates all originated from donkey jacks in France and the USA during 1997-2006. PAGE fractionated all of the 13 CRISPRs separated by 12 NRUSRs in T. equigenitalis EQ59. Permutation examples of CRISPRs, which were separated by NRUSRs for small-sized ladders, consisting of two doublet bands were shown. Putative CRISPRs separated by NRUSRs were amplified with 14/17 (82.4 %) geographically disparate T. equigenitalis isolates using the newly designed primer pair. Approximately 82.4 % of the T. equigenitalis isolates had CRISPRs separated by NRUSRs. The CRISPR locus was also found in the French T. asinigenitalis strain MCE3. Putative CRISPRs separated by NRUSRs were detected similarly in 4/14 (28.6 %) T. asinigenitalis isolates. Overall, a more detailed understanding of the molecular biology of CRISPRs within Taylorella organisms may help elucidate the pathogenic virulence and transmission mechanisms associated with this important equine pathogen.

Hydrodynamic injection with pneumatic valving for microchip electrophoresis with total analyte utilization

DOE Office of Scientific and Technical Information (OSTI.GOV)

Sun, Xuefei; Kelly, Ryan T.; Danielson, William F.

2011-04-26

A novel hydrodynamic injector that is directly controlled by a pneumatic valve has been developed for reproducible microchip capillary electrophoresis (CE) separations. The poly(dimethylsiloxane) (PDMS) devices used for evaluation comprise a separation channel, a side channel for sample introduction, and a pneumatic valve aligned at the intersection of the channels. A low pressure (≤ 3 psi) applied to the sample reservoir is sufficient to drive sample into the separation channel. The rapidly actuated pneumatic valve enables injection of discrete sample plugs as small as ~100 pL for CE separation. The injection volume can be easily controlled by adjusting the intersectionmore » geometry, the solution back pressure and the valve actuation time. Sample injection could be reliably operated at different frequencies (< 0.1 Hz to >2 Hz) with good reproducibility (peak height relative standard deviation ≤ 3.6%) and no sampling biases associated with the conventional electrokinetic injections. The separation channel was dynamically coated with a cationic polymer, and FITC-labeled amino acids were employed to evaluate the CE separation. Highly efficient (≥ 7.0 × 103 theoretical plates for the ~2.4 cm long channel) and reproducible CE separations were obtained. The demonstrated method has numerous advantages compared with the conventional techniques, including repeatable and unbiased injections, no sample waste, high duty cycle, controllable injected sample volume, and fewer electrodes with no need for voltage switching. The prospects of implementing this injection method for coupling multidimensional separations, for multiplexing CE separations and for sample-limited bioanalyses are discussed.« less

Identification and Structure Elucidation of Forced Degradation Products of the Novel Propionic acid Derivative Loxoprofen: Development of Stability-Indicating Chromatographic Methods Validated as per ICH Guidelines.

PubMed

Eissa, Maya S; Abd El-Sattar, Osama I

2017-04-01

Loxoprofen sodium (LOX) is a recently developed novel propionic acid derivative. Owing to its instability under both hydrolytic and oxidative conditions, the development of simple, rapid and sensitive methods for its determination in the presence of its possible forced degradation products becomes essential. Two simple chromatographic methods, high-performance thin layer chromatography (HPTLC) and high-performance liquid chromatography (HPLC), were developed associated with ultraviolet (UV) detection. In HPTLC-densitometric method, the separation of LOX from its degradation products was achieved using silica gel F254 plates and toluene:acetone:acetic acid (1.8:1.0:0.1, v/v/v) as the developing system followed by densitometric scanning at 220 nm. In the HPLC-UV method, the separation was performed using isocratic elution system with acetonitrile: 0.15% triethylamine (pH 2.2) (50:50, v/v) on C18 analytical column. The flow rate was optimized at 1.0 mL·min-1 and UV detection was achieved at 220 nm. Validation was performed in accordance with the International Conference on Harmonization guidelines and the method was perfectly applied for determination of LOX in its pharmaceutical preparation. The results obtained were statistically compared to those obtained after application of the official HPLC method, where no significant difference was found incompliance with precision and accuracy. Identification and characterization of the possible hydrolytic degradation product under alkaline conditions and that produced during oxidative degradation using hydrogen peroxide were structurally elucidated using infrared and mass spectrometry analyses. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Liu, Ying

My graduate research has focused on separation science and bioanalytical analysis, which emphasized in method development. It includes three major areas: enantiomeric separations using high performance liquid chromatography (HPLC), Super/subcritical fluid chromatography (SFC), and capillary electrophoresis (CE); drug-protein binding behavior studies using CE; and carbohydrate analysis using liquid chromatograph-electrospray ionization mass spectrometry (LC-ESI-MS). Enantiomeric separations continue to be extremely important in the pharmaceutical industry. An in-depth evaluation of the enantiomeric separation capabilities of macrocyclic glycopeptides CSPs with SFC mobile phases was investigated using a set of over 100 chiral compounds. It was found that the macrocyclic based CSPs were ablemore » to separate enantiomers of various compounds with different polarities and functionalities. Seventy percent of all separations were achieved in less than 4 min due to the high flow rate (4.0 ml/min) that can be used in SFC. Drug-protein binding is an important process in determining the activity and fate of a drug once it enters the body. Two drug/protein systems have been studied using frontal analysis CE method. More sensitive fluorescence detection was introduced in this assay, which overcame the problem of low sensitivity that is common when using UV detection for drug-protein studies. In addition, the first usage of an argon ion laser with 257 nm beam coupled with CCD camera as a frontal analysis detection method enabled the simultaneous observation of drug fluorescence as well as the protein fluorescence. LC-ESI-MS was used for the separation and characterization of underivatized oligosaccharide mixtures. With the limits of detection as low as 50 picograms, all individual components of oligosaccharide mixtures (up to 11 glucose-units long) were baseline resolved on a Cyclobond I 2000 column and detected using ESI-MS. This system is characterized by high chromatographic resolution, high column stability, and high sensitivity. In addition, this method showed potential usefulness for the sensitive and quick analysis of hydrolysis products of polysaccharides, and for trace level analysis of individual oligosaccharides or oligosaccharide isomers from biological systems.« less

A Facile Method for Separating and Enriching Nano and Submicron Particles from Titanium Dioxide Found in Food and Pharmaceutical Products.

PubMed

Faust, James J; Doudrick, Kyle; Yang, Yu; Capco, David G; Westerhoff, Paul

2016-01-01

Recent studies indicate the presence of nano-scale titanium dioxide (TiO2) as an additive in human foodstuffs, but a practical protocol to isolate and separate nano-fractions from soluble foodstuffs as a source of material remains elusive. As such, we developed a method for separating the nano and submicron fractions found in commercial-grade TiO2 (E171) and E171 extracted from soluble foodstuffs and pharmaceutical products (e.g., chewing gum, pain reliever, and allergy medicine). Primary particle analysis of commercial-grade E171 indicated that 54% of particles were nano-sized (i.e., < 100 nm). Isolation and primary particle analysis of five consumer goods intended to be ingested revealed differences in the percent of nano-sized particles from 32%‒58%. Separation and enrichment of nano- and submicron-sized particles from commercial-grade E171 and E171 isolated from foodstuffs and pharmaceuticals was accomplished using rate-zonal centrifugation. Commercial-grade E171 was separated into nano- and submicron-enriched fractions consisting of a nano:submicron fraction of approximately 0.45:1 and 3.2:1, respectively. E171 extracted from gum had nano:submicron fractions of 1.4:1 and 0.19:1 for nano- and submicron-enriched, respectively. We show a difference in particle adhesion to the cell surface, which was found to be dependent on particle size and epithelial orientation. Finally, we provide evidence that E171 particles are not immediately cytotoxic to the Caco-2 human intestinal epithelium model. These data suggest that this separation method is appropriate for studies interested in isolating the nano-sized particle fraction taken directly from consumer products, in order to study separately the effects of nano and submicron particles.

A Facile Method for Separating and Enriching Nano and Submicron Particles from Titanium Dioxide Found in Food and Pharmaceutical Products

PubMed Central

Yang, Yu; Capco, David G.; Westerhoff, Paul

2016-01-01

Recent studies indicate the presence of nano-scale titanium dioxide (TiO2) as an additive in human foodstuffs, but a practical protocol to isolate and separate nano-fractions from soluble foodstuffs as a source of material remains elusive. As such, we developed a method for separating the nano and submicron fractions found in commercial-grade TiO2 (E171) and E171 extracted from soluble foodstuffs and pharmaceutical products (e.g., chewing gum, pain reliever, and allergy medicine). Primary particle analysis of commercial-grade E171 indicated that 54% of particles were nano-sized (i.e., < 100 nm). Isolation and primary particle analysis of five consumer goods intended to be ingested revealed differences in the percent of nano-sized particles from 32%‒58%. Separation and enrichment of nano- and submicron-sized particles from commercial-grade E171 and E171 isolated from foodstuffs and pharmaceuticals was accomplished using rate-zonal centrifugation. Commercial-grade E171 was separated into nano- and submicron-enriched fractions consisting of a nano:submicron fraction of approximately 0.45:1 and 3.2:1, respectively. E171 extracted from gum had nano:submicron fractions of 1.4:1 and 0.19:1 for nano- and submicron-enriched, respectively. We show a difference in particle adhesion to the cell surface, which was found to be dependent on particle size and epithelial orientation. Finally, we provide evidence that E171 particles are not immediately cytotoxic to the Caco-2 human intestinal epithelium model. These data suggest that this separation method is appropriate for studies interested in isolating the nano-sized particle fraction taken directly from consumer products, in order to study separately the effects of nano and submicron particles. PMID:27798677

A point vortex model for the formation of ocean eddies by flow separation

NASA Astrophysics Data System (ADS)

Southwick, O. R.; Johnson, E. R.; McDonald, N. R.

2015-01-01

A simple model for the formation of ocean eddies by flow separation from sharply curved horizontal boundary topography is developed. This is based on the Brown-Michael model for two-dimensional vortex shedding, which is adapted to more realistically model mesoscale oceanic flow by including a deforming free surface. With a free surface, the streamfunction for the flow is not harmonic so the conformal mapping methods used in the standard Brown-Michael approach cannot be used and the problem must be solved numerically. A numerical scheme is developed based on a Chebyshev spectral method for the streamfunction partial differential equation and a second order implicit timestepping scheme for the vortex position ordinary differntial equations. This method is used to compute shed vortex trajectories for three background flows: (A) a steady flow around a semi-infinite plate, (B) a free vortex moving around a semi-infinite plate, and (C) a free vortex moving around a right-angled wedge. In (A), the inclusion of surface deformation dramatically slows the vortex and changes its trajectory from a straight path to a curved one. In (B) and (C), without the inclusion of flow separation, free vortices traverse fully around the tip along symmetrical trajectories. With the effects of flow separation included, very different trajectories are found: for all values of the model parameter—the Rossby radius—the free and shed vortices pair up and move off to infinity without passing around the tip. Their final propagation angle depends strongly and monotonically on the Rossby radius.

Development and validation of LC methods for the separation of misoprostol related substances and diastereoisomers.

PubMed

Kahsay, Getu; Song, Huiying; Eerdekens, Fran; Tie, Yaxin; Hendriks, Danny; Van Schepdael, Ann; Cabooter, Deirdre; Adams, Erwin

2015-01-01

Misoprostol is a synthetic prostaglandin E1 analogue which is mainly used for prevention and treatment of gastric ulcers, but also for abortion due to its labour inducing effect. Misoprostol exists as a mixture of diastereoisomers (1:1) and has several related impurities owing to its instability at higher temperatures and moisture. A simple and robust reversed phase liquid chromatographic (RPLC) method is described for the separation of the related substances and a normal phase (NP) LC method for the separation of misoprostol diastereoisomers. The RPLC method was performed using an Ascentis Express C18 (150 mm × 4.6 mm, 5 μm) column kept at 35 °C. The mobile phase was a gradient mixture of mobile phase A (ACN-H2O-MeOH, 28:69:3 v/v/v) and mobile phase B (ACN-H2O-MeOH, 47:50:3 v/v/v) eluted at a flow rate of 1.5 mL/min. UV detection was performed at 200 nm. The NPLC method was undertaken by using an XBridge bare silica (150 mm × 2.1 mm, 3.5 μm) column at 35 °C. The mobile phase contained 1-propanol-heptane-TFA (4:96:0.1%, v/v/v), pumped at a flow rate of 0.5 mL/min. UV detection was performed at 205 nm. This LC method can properly separate the two diastereoisomers (Rs > 2) within an analysis time of less than 20 min. Both methods were validated according to the ICH guidelines. Furthermore, these new LC methods have been successfully applied for purity control and diastereoisomers ratio determination of misoprostol bulk drug, tablets and dispersion. Copyright © 2015 Elsevier B.V. All rights reserved.

Quality by Design: Multidimensional exploration of the design space in high performance liquid chromatography method development for better robustness before validation.

PubMed

Monks, K; Molnár, I; Rieger, H-J; Bogáti, B; Szabó, E

2012-04-06

Robust HPLC separations lead to fewer analysis failures and better method transfer as well as providing an assurance of quality. This work presents the systematic development of an optimal, robust, fast UHPLC method for the simultaneous assay of two APIs of an eye drop sample and their impurities, in accordance with Quality by Design principles. Chromatography software is employed to effectively generate design spaces (Method Operable Design Regions), which are subsequently employed to determine the final method conditions and to evaluate robustness prior to validation. Copyright © 2011 Elsevier B.V. All rights reserved.

A method of evaluating crown fuels in forest stands.

Treesearch

Rodney W. Sando; Charles H. Wick

1972-01-01

A method of describing the crown fuels in a forest fuel complex based on crown weight and crown volume was developed. A computer program is an integral part of the method. Crown weight data are presented in graphical form and are separated into hardwood and coniferous fuels. The fuel complex is described using total crown weight per acre, mean height to the base of...

Stability-indicating chromatographic methods for the determination of some oxicams.

PubMed

Taha, Elham Anwer; Salama, Nahla Nour; Abdel Fattah, Laila el-Said

2004-01-01

Two sensitive and selective methods were developed for the determination of some oxicams, namely, lornoxicam (LOX), tenoxicam (TEX), and meloxicam (MEX), in the presence of their alkaline degradation products. The first method is based on the thin-layer chromatographic separation of the 3 drugs from their alkaline degradation products, followed by densitometric measurement of the intact drug spots for LOX, TEX, and MEX at 380, 370, and 364 nm, respectively. The developing systems used for separation are ethyl acetate-methanol-26% ammonia (17 + 3 + 0.35, v/v/v) for LOX and TEX and chloroform-n-hexane-96.0% acetic acid (18 + 1 + 1, v/v/v) for MEX. The linear ranges were 0.25-6.0 microg/spot for LOX and TEX and 0.5-10 microg/spot for MEX, with mean recoveries of 99.80 +/- 1.32, 100.57 +/- 1.34, and 100.71 +/- 1.57%, respectively. The second method is based on the liquid chromatographic separation of the 3 drugs from their alkaline degradation products on a reversed-phase C18 column, using mobile phases of methanol-acetonitrile-acetate buffer, pH 4.6 (4.5 + 0.5 + 5.0, v/v/v) for LOX and MEX and methanol-acetonitrile-acetate buffer, pH 4.6 (1.9 + 0.1 + 3.0, v/v/v) for TEX at ambient temperature. Quantification is achieved by UV detection at 280 nm, based on peak area. The linear ranges were 0.5-20 microg/mL for LOX and TEX and 1.25-50 microg/mL for MEX, with mean recoveries of 99.81 +/- 1.01, 98.90 +/- 1.61, and 100.86 +/- 1.55%, respectively. The methods were validated according to guidelines of the International Conference on Harmonization. The developed methods were successfully applied to the determination of LOX, TEX, and MEX in bulk powder, laboratory-prepared mixtures containing different percentages of degradation products, and pharmaceutical dosage forms.

Fast method to compute scattering by a buried object under a randomly rough surface: PILE combined with FB-SA.

PubMed

Bourlier, Christophe; Kubické, Gildas; Déchamps, Nicolas

2008-04-01

A fast, exact numerical method based on the method of moments (MM) is developed to calculate the scattering from an object below a randomly rough surface. Déchamps et al. [J. Opt. Soc. Am. A23, 359 (2006)] have recently developed the PILE (propagation-inside-layer expansion) method for a stack of two one-dimensional rough interfaces separating homogeneous media. From the inversion of the impedance matrix by block (in which two impedance matrices of each interface and two coupling matrices are involved), this method allows one to calculate separately and exactly the multiple-scattering contributions inside the layer in which the inverses of the impedance matrices of each interface are involved. Our purpose here is to apply this method for an object below a rough surface. In addition, to invert a matrix of large size, the forward-backward spectral acceleration (FB-SA) approach of complexity O(N) (N is the number of unknowns on the interface) proposed by Chou and Johnson [Radio Sci.33, 1277 (1998)] is applied. The new method, PILE combined with FB-SA, is tested on perfectly conducting circular and elliptic cylinders located below a dielectric rough interface obeying a Gaussian process with Gaussian and exponential height autocorrelation functions.

[Continual improvement of quantitative analytical method development of Panax notogineng saponins based on quality by design].

PubMed

Dai, Sheng-Yun; Xu, Bing; Shi, Xin-Yuan; Xu, Xiang; Sun, Ying-Qiang; Qiao, Yan-Jiang

2017-03-01

This study is aimed to propose a continual improvement strategy based on quality by design (QbD). An ultra high performance liquid chromatography (UPLC) method was developed to accomplish the method transformation from HPLC to UPLC of Panax notogineng saponins (PNS) and achieve the continual improvement of PNS based on QbD, for example. Plackett-Burman screening design and Box-Behnken optimization design were employed to further understand the relationship between the critical method parameters (CMPs) and critical method attributes (CMAs). And then the Bayesian design space was built. The separation degree of the critical peaks (ginsenoside Rg₁ and ginsenoside Re) was over 2.0 and the analysis time was less than 17 min by a method chosen from the design space with 20% of the initial concentration of the acetonitrile, 10 min of the isocratic time and 6%•min⁻¹ of the gradient slope. At last, the optimum method was validated by accuracy profile. Based on the same analytical target profile (ATP), the comparison of HPLC and UPLC including chromatograph method, CMA identification, CMP-CMA model and system suitability test (SST) indicated that the UPLC method could shorten the analysis time, improve the critical separation and satisfy the requirement of the SST. In all, HPLC method could be replaced by UPLC for the quantity analysis of PNS. Copyright© by the Chinese Pharmaceutical Association.

Basic features of boron isotope separation by SILARC method in the two-step iterative static model

NASA Astrophysics Data System (ADS)

Lyakhov, K. A.; Lee, H. J.

2013-05-01

In this paper we develop a new static model for boron isotope separation by the laser assisted retardation of condensation method (SILARC) on the basis of model proposed by Jeff Eerkens. Our model is thought to be adequate to so-called two-step iterative scheme for isotope separation. This rather simple model helps to understand combined action on boron separation by SILARC method of all important parameters and relations between them. These parameters include carrier gas, molar fraction of BCl3 molecules in carrier gas, laser pulse intensity, gas pulse duration, gas pressure and temperature in reservoir and irradiation cells, optimal irradiation cell and skimmer chamber volumes, and optimal nozzle throughput. A method for finding optimal values of these parameters based on some objective function global minimum search was suggested. It turns out that minimum of this objective function is directly related to the minimum of total energy consumed, and total setup volume. Relations between nozzle throat area, IC volume, laser intensity, number of nozzles, number of vacuum pumps, and required isotope production rate were derived. Two types of industrial scale irradiation cells are compared. The first one has one large throughput slit nozzle, while the second one has numerous small nozzles arranged in parallel arrays for better overlap with laser beam. It is shown that the last one outperforms the former one significantly. It is argued that NO2 is the best carrier gas for boron isotope separation from the point of view of energy efficiency and Ar from the point of view of setup compactness.

Experimental study of flow separation control on a low- Re airfoil using leading-edge protuberance method

NASA Astrophysics Data System (ADS)

Zhang, M. M.; Wang, G. F.; Xu, J. Z.

2014-04-01

An experimental study of flow separation control on a low- Re c airfoil was presently investigated using a newly developed leading-edge protuberance method, motivated by the improvement in the hydrodynamics of the giant humpback whale through its pectoral flippers. Deploying this method, the control effectiveness of the airfoil aerodynamics was fully evaluated using a three-component force balance, leading to an effectively impaired stall phenomenon and great improvement in the performances within the wide post-stall angle range (22°-80°). To understand the flow physics behind, the vorticity field, velocity field and boundary layer flow field over the airfoil suction side were examined using a particle image velocimetry and an oil-flow surface visualization system. It was found that the leading-edge protuberance method, more like low-profile vortex generator, effectively modified the flow pattern of the airfoil boundary layer through the chordwise and spanwise evolutions of the interacting streamwise vortices generated by protuberances, where the separation of the turbulent boundary layer dominated within the stall region and the rather strong attachment of the laminar boundary layer still existed within the post-stall region. The characteristics to manipulate the flow separation mode of the original airfoil indicated the possibility to further optimize the control performance by reasonably designing the layout of the protuberances.

Digital pulse shape discrimination methods for n-γ separation in an EJ-301 liquid scintillation detector

NASA Astrophysics Data System (ADS)

Wan, Bo; Zhang, Xue-Ying; Chen, Liang; Ge, Hong-Lin; Ma, Fei; Zhang, Hong-Bin; Ju, Yong-Qin; Zhang, Yan-Bin; Li, Yan-Yan; Xu, Xiao-Wei

2015-11-01

A digital pulse shape discrimination system based on a programmable module NI-5772 has been established and tested with an EJ-301 liquid scintillation detector. The module was operated by running programs developed in LabVIEW, with a sampling frequency up to 1.6 GS/s. Standard gamma sources 22Na, 137Cs and 60Co were used to calibrate the EJ-301 liquid scintillation detector, and the gamma response function was obtained. Digital algorithms for the charge comparison method and zero-crossing method have been developed. The experimental results show that both digital signal processing (DSP) algorithms can discriminate neutrons from γ-rays. Moreover, the zero-crossing method shows better n-γ discrimination at 80 keVee and lower, whereas the charge comparison method gives better results at higher thresholds. In addition, the figure-of-merit (FOM) for detectors of two different dimensions were extracted at 9 energy thresholds, and it was found that the smaller detector presented better n-γ separation for fission neutrons. Supported by National Natural Science Foundation of China (91226107, 11305229) and the Strategic Priority Research Program of the Chinese Academy of Sciences (XDA03030300)

Rapid purification of diastereoisomers from Piper kadsura using supercritical fluid chromatography with chiral stationary phases.

PubMed

Xin, Huaxia; Dai, Zhuoshun; Cai, Jianfeng; Ke, Yanxiong; Shi, Hui; Fu, Qing; Jin, Yu; Liang, Xinmiao

2017-08-04

Supercritical fluid chromatography (SFC) with chiral stationary phases (CSPs) is an advanced solution for the separation of achiral compounds in Piper kadsura. Analogues and stereoisomers are abundant in natural products, but there are obstacles in separation using conventional method. In this paper, four lignan diastereoisomers, (-)-Galbelgin, (-)-Ganschisandrin, Galgravin and (-)-Veraguensin, from Piper kadsura were separated and purified by chiral SFC. Purification strategy was designed, considering of the compound enrichment, sample purity and purification throughput. Two-step achiral purification method on chiral preparative columns with stacked automated injections was developed. Unconventional mobile phase modifier dichloromethane (DCM) was applied to improve the sample solubility. Four diastereoisomers was prepared at the respective weight of 103.1mg, 10.0mg, 152.3mg and 178.6mg from 710mg extract with the purity of greater than 98%. Copyright © 2017 Elsevier B.V. All rights reserved.

Liquid chromatographic separation of zalcitabine and its stereoisomers.

PubMed

Scypinski, S; Ross, A J

1994-10-01

A liquid chromatographic method capable of separating and quantitating the stereoisomers of zalcitabine has been developed and validated. The separation was achieved with an Astec Cyclobond I--RSP column and a mobile phase of 0.25% triethylamine in water adjusted to a pH of 6.5 with glacial acetic acid. All enantiomers were found to exhibit a linear response in the range of 0.1-10% in the presence of 100% zalcitabine. Precision of analysis was found to be less than 1.5% at a level of 1% relative to zalcitabine. The limit of detection for two of the three enantiomeric impurities was determined to be 0.05% relative to zalcitabine. The detection limit for the third was found to be 0.1%. This method was successfully applied to the analysis of reference standards and several production scale batches. All of these materials were found to be stereochemically pure to a level of 99.8% or better.

Identification of a parametric, discrete-time model of ankle stiffness.

PubMed

Guarin, Diego L; Jalaleddini, Kian; Kearney, Robert E

2013-01-01

Dynamic ankle joint stiffness defines the relationship between the position of the ankle and the torque acting about it and can be separated into intrinsic and reflex components. Under stationary conditions, intrinsic stiffness can described by a linear second order system while reflex stiffness is described by Hammerstein system whose input is delayed velocity. Given that reflex and intrinsic torque cannot be measured separately, there has been much interest in the development of system identification techniques to separate them analytically. To date, most methods have been nonparametric and as a result there is no direct link between the estimated parameters and those of the stiffness model. This paper presents a novel algorithm for identification of a discrete-time model of ankle stiffness. Through simulations we show that the algorithm gives unbiased results even in the presence of large, non-white noise. Application of the method to experimental data demonstrates that it produces results consistent with previous findings.

Efficient One-Step Electrolytic Recycling of Low-Grade and Post-Consumer Magnesium Scrap

DOE Office of Scientific and Technical Information (OSTI.GOV)

Adam C. Powell, IV

2012-07-19

Metal Oxygen Separation Technologies, Inc. (abbreviated MOxST, pronounced most) and Boston University (BU) have developed a new low-cost process for recycling post-consumer co-mingled and heavily-oxidized magnesium scrap, and discovered a new chemical mechanism for magnesium separations in the process. The new process, designated MagReGenTM, is very effective in laboratory experiments, and on scale-up promises to be the lowest-cost lowest-energy lowest-impact method for separating magnesium metal from aluminum while recovering oxidized magnesium. MagReGenTM uses as little as one-eighth as much energy as today's methods for recycling magnesium metal from comingled scrap. As such, this technology could play a vital role inmore » recycling automotive non-ferrous metals, particularly as motor vehicle magnesium/aluminum ratios increase in order to reduce vehicle weight and increase efficiency.« less

Separation of three water-soluble vitamins by poly(dimethylsiloxane) microchannel electrophoresis with electrochemical detection.

PubMed

Li, Xiang-Yun; Zhang, Qian-Li; Lian, Hong-Zhen; Xu, Jing-Juan; Chen, Hong-Yuan

2007-09-01

A method for rapid separation and sensitive determination of three water-soluble vitamins, pyridoxine, ascorbic acid (VC), and p-aminobenzoic acid (PABA) has been developed by PDMS microchannel electrophoresis integrated with amperometric detection. After treatment of the microchip with oxygen plasma, the peak shapes of the three analytes were essentially improved. Pyridoxine, VC, and PABA were well separated within only 80 s in a running buffer of 20 mM borate solution (pH 8.5). Good linearity was obtained within the concentration range of 2-200 microM for the three water-soluble vitamins. The detection limits were 1.0 microM for pyridoxine and VC, and 1.5 microM for PABA. The proposed method has been successfully applied to real human urine sample, without solid phase extraction, with recoveries of 80-122% for the three water-soluble vitamins.

Analysis of low molecular weight acids by monolithic immobilized pH gradient-based capillary isoelectric focusing coupled with mass spectrometry.

PubMed

Wang, Tingting; Fekete, Agnes; Gaspar, Andras; Ma, Junfeng; Liang, Zhen; Yuan, Huiming; Zhang, Lihua; Schmitt-Kopplin, Philippe; Zhang, Yukui

2011-02-01

A novel method for the separation and detection of low molecular weight (LMW) acids was developed using monolithic immobilized pH gradient-based capillary isoelectric focusing coupled with mass spectrometry. Two main parameters, focusing conditions and delivery buffer conditions, which might affect separation efficiency, were optimized with the focusing time of 7 min at 350 V/cm and the delivery buffer of 50% (v/v) acetonitrile in 10 mmol/L ammonium formate (pH 3.0). Under these conditions, the linear correlation between the volume of delivery solvent and the pK(a) of the model components was observed. In addition, the separation mechanism of LMW acids was proposed as well. We suppose that this method may provide a useful tool for the characterization of LMW components (e.g. natural organic matter of different origins). Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Systematic Development and Validation of a Thin-Layer Densitometric Bioanalytical Method for Estimation of Mangiferin Employing Analytical Quality by Design (AQbD) Approach.

PubMed

Khurana, Rajneet Kaur; Rao, Satish; Beg, Sarwar; Katare, O P; Singh, Bhupinder

2016-01-01

The present work aims at the systematic development of a simple, rapid and highly sensitive densitometry-based thin-layer chromatographic method for the quantification of mangiferin in bioanalytical samples. Initially, the quality target method profile was defined and critical analytical attributes (CAAs) earmarked, namely, retardation factor (Rf), peak height, capacity factor, theoretical plates and separation number. Face-centered cubic design was selected for optimization of volume loaded and plate dimensions as the critical method parameters selected from screening studies employing D-optimal and Plackett-Burman design studies, followed by evaluating their effect on the CAAs. The mobile phase containing a mixture of ethyl acetate : acetic acid : formic acid : water in a 7 : 1 : 1 : 1 (v/v/v/v) ratio was finally selected as the optimized solvent for apt chromatographic separation of mangiferin at 262 nm withRf 0.68 ± 0.02 and all other parameters within the acceptance limits. Method validation studies revealed high linearity in the concentration range of 50-800 ng/band for mangiferin. The developed method showed high accuracy, precision, ruggedness, robustness, specificity, sensitivity, selectivity and recovery. In a nutshell, the bioanalytical method for analysis of mangiferin in plasma revealed the presence of well-resolved peaks and high recovery of mangiferin. © The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Development and validation of a reversed phase liquid chromatographic method for analysis of oxytetracycline and related impurities.

PubMed

Kahsay, Getu; Shraim, Fairouz; Villatte, Philippe; Rotger, Jacques; Cassus-Coussère, Céline; Van Schepdael, Ann; Hoogmartens, Jos; Adams, Erwin

2013-03-05

A simple, robust and fast high-performance liquid chromatographic method is described for the analysis of oxytetracycline and its related impurities. The principal peak and impurities are all baseline separated in 20 min using an Inertsil C₈ (150 mm × 4.6 mm, 5 μm) column kept at 50 °C. The mobile phase consists of a gradient mixture of mobile phases A (0.05% trifluoroacetic acid in water) and B (acetonitrile-methanol-tetrahydrofuran, 80:15:5, v/v/v) pumped at a flow rate of 1.3 ml/min. UV detection was performed at 254 nm. The developed method was validated for its robustness, sensitivity, precision and linearity in the range from limit of quantification (LOQ) to 120%. The limits of detection (LOD) and LOQ were found to be 0.08 μg/ml and 0.32 μg/ml, respectively. This method allows the separation of oxytetracycline from all known and 5 unknown impurities, which is better than previously reported in the literature. Moreover, the simple mobile phase composition devoid of non-volatile buffers made the method suitable to interface with mass spectrometry for further characterization of unknown impurities. The developed method has been applied for determination of related substances in oxytetracycline bulk samples available from four manufacturers. The validation results demonstrate that the method is reliable for quantification of oxytetracycline and its impurities. Copyright © 2012 Elsevier B.V. All rights reserved.

Development and validation of a liquid chromatography-tandem mass spectrometry method for the separation of conjugated and unconjugated 17alpha- and 17beta-boldenone in urine sample.

PubMed

Gasparini, Mara; Assini, Walter; Bozzoni, Eros; Tognoli, Nadia; Dusi, Guglielmo

2007-03-14

Natural occurrence or illegal treatment of boldenone (BOLD) presence in cattle urine is under debate within the European Union. Separation of conjugated and unconjugated forms of 17alpha-boldenone (alpha-BOLD) and 17beta-boldenone (beta-BOLD) and presence of related molecules as androsta-1,4-diene-3,17-dione (ADD) appear critical points for the decision of an illegal use. The aim of this study is a new analytical approach of BOLD and ADD confirmation in cattle urine. The separation between conjugated and unconjugated forms of BOLD was obtained by a preliminary urine liquid-liquid extraction step with ethyl acetate. In this step the organic phase extracts only unconjugated BOLD and ADD, while BOLD in conjugated form remain in urine phase. Afterwards the urine phase, contains conjugated BOLD, was subjected to an enzymatic deconjugation. Solid-phase extraction (OASIS-HLB Waters) was used for the purification and concentration of analytes in organic and urine phases and liquid chromatography ion electrospray tandem mass spectrometry (LC-MS-MS) was applied for the confirmation of BOLD and ADD, using deuterium-labelled 17beta-boldenone (BOLD-d3) as internal standard. The method was validated as a quantitative confirmatory method according to the Commission Decision 2002/657/CE. The results obtained demonstrate that the developed method show very high specificity, precision, trueness and ruggedness. Decision limits (CCalpha) smaller than 0.5 ng mL(-1) were obtained for each analyte.

Determination of antioxidants by a novel on-line HPLC-cupric reducing antioxidant capacity (CUPRAC) assay with post-column detection.

PubMed

Celik, Saliha Esin; Ozyürek, Mustafa; Güçlü, Kubilay; Apak, Reşat

2010-07-26

A novel on-line HPLC-cupric reducing antioxidant capacity (CUPRAC) method was developed for the selective determination of polyphenols (flavonoids, simple phenolic and hydroxycinnamic acids) in complex plant matrices. The method combines chromatographic separation, constituent analysis, and post-column identification of antioxidants in plant extracts. The separation of polyphenols was performed on a C18 column using gradient elution with two different mobile phase solutions, i.e., MeOH and 0.2% o-phosphoric acid. The HPLC-separated antioxidant polyphenols in the extracts react with copper(II)-neocuproine (Cu(II)-Nc) reagent in a post-column reaction coil to form a derivative. The reagent is reduced by antioxidants to the copper(I)-neocuproine (Cu(I)-Nc) chelate having maximum absorption at 450 nm. The negative peaks of antioxidant constituents were monitored by measuring the increase in absorbance due to Cu(I)-Nc. The detection limits of polyphenols at 450 nm (in the range of 0.17-3.46 microM) after post-column derivatization were comparable to those at 280 nm UV detection without derivatization. The developed method was successfully applied to the identification of antioxidant compounds in crude extracts of Camellia sinensis, Origanum marjorana and Mentha. The method is rapid, inexpensive, versatile, non-laborious, uses stable reagents, and enables the on-line qualitative and quantitative estimation of antioxidant constituents of complex plant samples. Copyright 2010 Elsevier B.V. All rights reserved.

Rapid Detection and Enumeration of Giardia lamblia Cysts in Water Samples by Immunomagnetic Separation and Flow Cytometric Analysis ▿ †

PubMed Central

Keserue, Hans-Anton; Füchslin, Hans Peter; Egli, Thomas

2011-01-01

Giardia lamblia is an important waterborne pathogen and is among the most common intestinal parasites of humans worldwide. Its fecal-oral transmission leads to the presence of cysts of this pathogen in the environment, and so far, quantitative rapid screening methods are not available for various matrices, such as surface waters, wastewater, or food. Thus, it is necessary to establish methods that enable reliable rapid detection of a single cyst in 10 to 100 liters of drinking water. Conventional detection relies on cyst concentration, isolation, and confirmation by immunofluorescence microscopy (IFM), resulting in low recoveries and high detection limits. Many different immunomagnetic separation (IMS) procedures have been developed for separation and cyst purification, so far with variable but high losses of cysts. A method was developed that requires less than 100 min and consists of filtration, resuspension, IMS, and flow cytometric (FCM) detection. MACS MicroBeads were used for IMS, and a reliable flow cytometric detection approach was established employing 3 different parameters for discrimination from background signals, i.e., green and red fluorescence (resulting from the distinct pattern emitted by the fluorescein dye) and sideward scatter for size discrimination. With spiked samples, recoveries exceeding 90% were obtained, and false-positive results were never encountered for negative samples. Additionally, the method was applicable to naturally occurring cysts in wastewater and has the potential to be automated. PMID:21685159

The separate universe approach to soft limits

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kenton, Zachary; Mulryne, David J., E-mail: z.a.kenton@qmul.ac.uk, E-mail: d.mulryne@qmul.ac.uk

We develop a formalism for calculating soft limits of n -point inflationary correlation functions using separate universe techniques. Our method naturally allows for multiple fields and leads to an elegant diagrammatic approach. As an application we focus on the trispectrum produced by inflation with multiple light fields, giving explicit formulae for all possible single- and double-soft limits. We also investigate consistency relations and present an infinite tower of inequalities between soft correlation functions which generalise the Suyama-Yamaguchi inequality.

Hydrophilic interaction liquid chromatography for the separation, purification, and quantification of raffinose family oligosaccharides from Lycopus lucidus Turcz.

PubMed

Liang, Tu; Fu, Qing; Li, Fangbing; Zhou, Wei; Xin, Huaxia; Wang, Hui; Jin, Yu; Liang, Xinmiao

2015-08-01

A systematic strategy based on hydrophilic interaction liquid chromatography was developed for the separation, purification and quantification of raffinose family oligosaccharides from Lycopus lucidus Turcz. Methods with enough hydrophilicity and selectivity were utilized to resolve the problems encountered in the separation of oligosaccharides such as low retention, low resolution and poor solubility. The raffinose family oligosaccharides in L. lucidus Turcz. were isolated using solid-phase extraction followed by hydrophilic interaction liquid chromatography at semi-preparative scale to obtain standards of stachyose, verbascose and ajugose. Utilizing the obtained oligosaccharides as standards, a quantitative determination method was developed, validated and applied for the content determination of raffinose family oligosaccharides both in the aerial and root parts of L. lucidus Turcz. There were no oligosaccharides in the aerial parts, while in the root parts, the total content was 686.5 mg/g with the average distribution: raffinose 66.5 mg/g, stachyose 289.0 mg/g, verbascose 212.4 mg/g, and ajugose 118.6 mg/g. The result provided the potential of roots of L. lucidus Turcz. as new raffinose family oligosaccharides sources for functional food. Moreover, since the present systematic strategy is efficient, sensitive and robust, separation, purification and quantification of oligosaccharides by hydrophilic interaction liquid chromatography seems to be possible. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Development and validation of a single robust HPLC method for the characterization of a pharmaceutical starting material and impurities from three suppliers using three separate synthetic routes.

PubMed

Sheldon, E M; Downar, J B

2000-08-15

Novel approaches to the development of analytical procedures for monitoring incoming starting material in support of chemical/pharmaceutical processes are described. High technology solutions were utilized for timely process development and preparation of high quality clinical supplies. A single robust HPLC method was developed and characterized for the analysis of the key starting material from three suppliers. Each supplier used a different process for the preparation of this material and, therefore, each suppliers' material exhibited a unique impurity profile. The HPLC method utilized standard techniques acceptable for release testing in a QC/manufacturing environment. An automated experimental design protocol was used to characterize the robustness of the HPLC method. The method was evaluated for linearity, limit of quantitation, solution stability, and precision of replicate injections. An LC-MS method that emulated the release HPLC method was developed and the identities of impurities were mapped between the two methods.

A Physicochemical Method for Separating Rare Earths: Addressing an Impending Shortfall

DOE Office of Scientific and Technical Information (OSTI.GOV)

Schelter, Eric

2017-03-14

There are currently zero operating suppliers of critical rare earth elements La–Lu, Sc, Y (REs), in the western hemisphere. REs are critical materials due to their importance in clean energy and defense applications, including permanent magnets in wind turbines and phosphors in energy efficient lighting. It is not economically viable to produce pure REs in the U.S. given current separations technology. REs production is dominated by suppliers in the People’s Republic of China (PRC) because of their capacity in liquid­liquid solvent extraction (SX) used to purify mixtures. Weak environmental regulations in the PRC also contribute to a competitive advantage. SXmore » is a cost, time, solvent and waste intensive process but is highly optimized and scalable. The low efficiency of SX derives from the small thermodynamic differences in solvation enthalpy between the RE3+ cations. To foster stable domestic RE production there is a critical need for fundamentally new REs chemistry that contributes to disruptive technologies in RE separations. The overall goal of this project was to develop new thermodynamic bases, and apply them, for the solution separation of rare earth metals. We have developed the chemistry of rare earth metals: La–Lu, Sc and Y, with redox active ligands. Our hypothesis for the project was that electron­hole coupling in complexes of certain lanthanide metals with redox active ligands can be used to manifest chemical distinctiveness and affect separations. We also developed separations based on unique solution equilibria from tailored ligands.« less

Overview of Transonic to Hypersonic Stage Separation Tool Development for Multi-Stage-to-Orbit Concepts

NASA Technical Reports Server (NTRS)

Murphy, Kelly J.; Bunning, Pieter G.; Pamadi, Bandu N.; Scallion, William I.; Jones, Kenneth M.

2004-01-01

An overview of research efforts at NASA in support of the stage separation and ascent aerothermodynamics research program is presented. The objective of this work is to develop a synergistic suite of experimental, computational, and engineering tools and methods to apply to vehicle separation across the transonic to hypersonic speed regimes. Proximity testing of a generic bimese wing-body configuration is on-going in the transonic (Mach numbers 0.6, 1.05, and 1.1), supersonic (Mach numbers 2.3, 3.0, and 4.5) and hypersonic (Mach numbers 6 and 10) speed regimes in four wind tunnel facilities at the NASA Langley Research Center. An overset grid, Navier-Stokes flow solver has been enhanced and demonstrated on a matrix of proximity cases and on a dynamic separation simulation of the bimese configuration. Steady-state predictions with this solver were in excellent agreement with wind tunnel data at Mach 3 as were predictions via a Cartesian-grid Euler solver. Experimental and computational data have been used to evaluate multi-body enhancements to the widely-used Aerodynamic Preliminary Analysis System, an engineering methodology, and to develop a new software package, SepSim, for the simulation and visualization of vehicle motions in a stage separation scenario. Web-based software will be used for archiving information generated from this research program into a database accessible to the user community. Thus, a framework has been established to study stage separation problems using coordinated experimental, computational, and engineering tools.

Superhydrophobic hierarchical structure carbon mesh films for oil/water separation application

NASA Astrophysics Data System (ADS)

Lu, Zhaoxia; Huang, Xing; Wang, Lisheng

2017-08-01

In this study, we showed that a superoleophobic mesh with the self-cleaning ability could be readily prepared by a facile spray-coating method on stainless steel mesh. Poly(methyl methacrylate) was employed to provide a stable strength between carbon nanotubes and steel mesh surface. The effect of opening size of these steel meshes on surface wetting has been investigated. The dynamics of liquid droplets was investigated as well. The as-prepared meshes exhibited both superhydrophobicity and superoleophilicity and could effectively separate water from the oil and water mixture. The present study contributes to the development of oil and water separation materials for marine industrial application.