ELECTROSTRICTION VALVE

DOEpatents

Kippenhan, D.O.

1962-09-25

An accurately controlled, pulse gas valve is designed capable of delivering output pulses which vary in length from one-tenth millisecond to one second or more, repeated at intervals of a few milliseconds or- more. The pulsed gas valve comprises a column formed of barium titanate discs mounted in stacked relation and electrically connected in parallel, with means for applying voltage across the discs to cause them to expand and effect a mechanical elongation axially of the column. The column is mounted within an enclosure having an inlet port and an outlet port with an internal seat in communication with the outlet port, such that a plug secured to the end of the column will engage the seat of the outlet port to close the outlet port in response to the application of voltage is regulated by a conventional electronic timing circuit connected to the column. (AEC)

Nondestructive evaluation of the preservation state of stone columns in the Hospital Real of Granada

NASA Astrophysics Data System (ADS)

Moreno de Jong van Coevorden, C.; Cobos Sánchez, C.; Rubio Bretones, A.; Fernández Pantoja, M.; García, Salvador G.; Gómez Martín, R.

2012-12-01

This paper describes the results of the employment of two nondestructive evaluation methods for the diagnostic of the preservation state of stone elements. The first method is based on ultrasonic (US) pulses while the second method uses short electromagnetic pulses. Specifically, these methods were applied to some columns, some of them previously restored. These columns are part of the architectonic heritage of the University of Granada, in particular they are located at the patio de la capilla del Hospital Real of Granada. The objective of this work was the application of systems based on US pulses (in transmission mode) and the ground-penetrating radar systems (electromagnetic tomography) in the diagnosis and detection of possible faults in the interior of columns.

Column CO2 Measurement From an Airborne Solid-State Double-Pulsed 2-Micron Integrated Path Differential Absorption Lidar

NASA Technical Reports Server (NTRS)

Singh, U. N.; Yu, J.; Petros, M.; Refaat, T. F.; Remus, R.; Fay, J.; Reithmaier, K.

2014-01-01

NASA LaRC is developing and integrating a double-Pulsed 2-micron direct detection IPDA lidar for CO2 column measurement from an airborne platform. The presentation will describe the development of the 2-micrometers IPDA lidar system and present the airborne measurement of column CO2 and will compare to in-situ measurement for various ground target of different reflectivity.

Effect of pressure pulses at the interface valve on the stability of second dimension columns in online comprehensive two-dimensional liquid chromatography.

PubMed

Talus, Eric S; Witt, Klaus E; Stoll, Dwight R

2015-01-23

Users of online comprehensive two-dimensional liquid chromatography (LCxLC) frequently acknowledge that the mechanical instability of HPLC columns installed in these systems, particularly in the second dimension, is a significant impediment to its use. Such instability is not surprising given the strenuous operating environment to which these columns are subjected, including the large number (thousands per day) of fast and large pressure pulses resulting from interface valve switches (on the timescale of tens of milliseconds) associated with very fast second dimension separations. There appear to be no published reports of systematic studies of the relationship between second dimension column lifetime and any of these variables. In this study we focused on the relationship between the lifetimes of commercially available columns and the pressure pulses observed at the inlet of the second dimension column that occur during the switching of the valve that interfaces the two dimensions of a LCxLC system. We find that the magnitude of the pressure drop at the inlet of the second dimension column during the valve switch, which may vary between 10 and 95% of the column inlet pressure, is dependent on valve switching speed and design, and has a dramatic impact on column lifetime. In the worst case, columns fail within the first few hours of use in an LCxLC system. In the best case, using a valve that exhibits much smaller pressure pulses, the same columns exhibit much improved lifetimes and have been used continuously under LCxLC conditions for several days with no degradation in performance. This result represents a first step in understanding the factors that affect second dimension column lifetime, and will significantly improve the usability of the LCxLC technique in general. Copyright © 2014 Elsevier B.V. All rights reserved.

Pulsed electric field processing for fruit and vegetables

USDA-ARS?s Scientific Manuscript database

This month’s column reviews the theory and current applications of pulsed electric field (PEF) processing for fruits and vegetables to improve their safety and quality. This month’s column coauthor, Stefan Toepfl, is advanced research manager at the German Institute of Food Technologies and professo...

Airborne 2-Micron Double-Pulsed Integrated Path Differential Absorption Lidar for Column CO2 Measurement

NASA Technical Reports Server (NTRS)

Singh, Upendra N.; Yu, Jirong; Petros, Mulugeta; Refaat, Tamer F.; Remus, Ruben G.; Fay, James J.; Reithmaier, Karl

2014-01-01

Double-pulse 2-micron lasers have been demonstrated with energy as high as 600 millijouls and up to 10 Hz repetition rate. The two laser pulses are separated by 200 microseconds and can be tuned and locked separately. Applying double-pulse laser in DIAL system enhances the CO2 measurement capability by increasing the overlap of the sampled volume between the on-line and off-line. To avoid detection complicity, integrated path differential absorption (IPDA) lidar provides higher signal-to-noise ratio measurement compared to conventional range-resolved DIAL. Rather than weak atmospheric scattering returns, IPDA rely on the much stronger hard target returns that is best suited for airborne platforms. In addition, the IPDA technique measures the total integrated column content from the instrument to the hard target but with weighting that can be tuned by the transmitter. Therefore, the transmitter could be tuned to weight the column measurement to the surface for optimum CO2 interaction studies or up to the free troposphere for optimum transport studies. Currently, NASA LaRC is developing and integrating a double-Pulsed 2-micron direct detection IPDA lidar for CO2 column measurement from an airborne platform. The presentation will describe the development of the 2-micron IPDA lidar system and present the airborne measurement of column CO2 and will compare to in-situ measurement for various ground target of different reflectivity.

Use of mesophilic and thermophilic bacteria for the improvement of copper extraction from a low-grade ore

NASA Astrophysics Data System (ADS)

Darezereshki, E.; Schaffie, M.; Lotfalian, M.; Seiedbaghery, S. A.; Ranjbar, M.

2011-04-01

Bioleaching was examined for copper extraction from a low grade ore using mesophilic and moderate thermophilic bacteria. Five equal size columns were used for the leaching of the ore. Sulfuric acid solution with a flow rate of 3.12 L·m-2·h-1 and pH 1.5 passed through each column continuously for 90 d. In the first and the second column, bioleaching was performed without agglomeration of the ore and on the agglomerated ore, respectively. 28wt% of the copper was extracted in the first column after 40 d, while this figure was 38wt% in the second column. After 90 d, however, the overall extractions were almost the same for both of them. Bioleaching with mesophilic bacteria was performed in the third column without agglomeration of the ore and in the fourth column on the agglomerated ore. After 40 d, copper extractions in the third and the fourth columns were 62wt% and 70wt%, respectively. Copper extractions were 75wt% for both the columns after 90 d. For the last column, bioleaching was performed with moderate thermophilic bacteria and agglomerated ore. Copper extractions were 80wt% and 85wt% after 40 and 90 d, respectively. It was concluded that crushing and agglomeration of the ore using bacteria could enhance the copper extraction considerably.

Increasing Flexibility in Two-Dimensional Liquid Chromatography by Pulsed Elution of the First Dimension: A Proof of Concept.

PubMed

Jakobsen, Simon S; Christensen, Jan H; Verdier, Sylvain; Mallet, Claude R; Nielsen, Nikoline J

2017-09-05

This work demonstrates the development of an online two-dimensional liquid chromatography (2D-LC) method where the first dimension column is eluted by a sequence of pulses of increasing eluotropic strength generated by the LC pumps (pulsed-elution 2D-LC). Between the pulses, the first dimension is kept in a no-elution state using low eluent strength. The eluate from the first dimension is actively modulated using trap columns and subsequently analyzed in the second dimension. We demonstrate that by tuning the length and eluotropic strength of the pulses, peaks with retention factors in water, k w , above 150 can be manipulated to elute in 3-4 pulses. The no-elution state can be kept for 1-10 min with only minor changes as to which and how many pulses the peaks elute in. Pulsed-elution 2D-LC combined with active modulation tackles three of the main challenges encountered in 2D-LC and specifically online comprehensive 2D-LC: undersampling, difficulties in refocusing, and lack of flexibility in the selection of column dimensions and flow rates because the two dimensions constrain each other. The pulsed-elution 2D-LC was applied for the analysis of a basic fraction of vacuum gas oil. Peak capacity was 4018 for a 540 min analysis and 4610 for a 1040 min analysis.

10 CFR Appendix E to Part 110 - Illustrative List of Chemical Exchange or Ion Exchange Enrichment Plant Equipment and Components...

Code of Federal Regulations, 2011 CFR

2011-01-01

... contactors employed in the separation cascade can be liquid-liquid exchange columns (such as pulsed columns.... Plastic, plastic-lined (including use of fluorocarbon polymers) and/or glass-lined columns and piping are therefore used. (1) Liquid-liquid exchange columns. Countercurrent liquid-liquid exchange columns having...

10 CFR Appendix E to Part 110 - Illustrative List of Chemical Exchange or Ion Exchange Enrichment Plant Equipment and Components...

Code of Federal Regulations, 2013 CFR

2013-01-01

... contactors employed in the separation cascade can be liquid-liquid exchange columns (such as pulsed columns.... Plastic, plastic-lined (including use of fluorocarbon polymers) and/or glass-lined columns and piping are therefore used. (1) Liquid-liquid exchange columns. Countercurrent liquid-liquid exchange columns having...

10 CFR Appendix E to Part 110 - Illustrative List of Chemical Exchange or Ion Exchange Enrichment Plant Equipment and Components...

Code of Federal Regulations, 2014 CFR

2014-01-01

... contactors employed in the separation cascade can be liquid-liquid exchange columns (such as pulsed columns.... Plastic, plastic-lined (including use of fluorocarbon polymers) and/or glass-lined columns and piping are therefore used. (1) Liquid-liquid exchange columns. Countercurrent liquid-liquid exchange columns having...

Trip report. Eurochemic company assistance: Hanford Atomic Products Operation spent fuel processing technology

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

Shank, E.M.

1959-06-23

Information obtained from HAPO during visit by M.K. Twichell, UCNC, and E.M. Shank, ORNL, is given. Included are the tentative procedures for obtaining and transmitting information to the Eurochemic company. Discussions are given on pulsed columns, corrosion, puse generators, centrifuges, valves, in-line instrumentation, evaporators, resin column design, off-gas processing, solvent recovery, liquid-waste handling, process control, equipment decontamination, criticality, radiation protection, diluent, and solvent stability, backmixing in a pulsed column, and use of 40% TBP in the purex flowsheet.

The study on the extraction method of indirubin from Indigo Naturalis.

PubMed

Cheng, Li-hui

2007-01-01

To discuss how to extract the indirubin of the higher purity from Indigo Naturalis. After extracting the indirubin from Indigo Naturalis by acetic ether, compare the separation effect of the extract in Si gel column with that in alumina column. The indirubin in Indigo Naturalis by Si gel column chromatography is chosen. The purity of indirubin is 98.3% after Si gel column chromatography. The indiruhbin of the higher purity was attained by the simple experimental method.

Highly-Integrated CMOS Interface Circuits for SiPM-Based PET Imaging Systems.

PubMed

Dey, Samrat; Lewellen, Thomas K; Miyaoka, Robert S; Rudell, Jacques C

2012-01-01

Recent developments in the area of Positron Emission Tomography (PET) detectors using Silicon Photomultipliers (SiPMs) have demonstrated the feasibility of higher resolution PET scanners due to a significant reduction in the detector form factor. The increased detector density requires a proportionally larger number of channels to interface the SiPM array with the backend digital signal processing necessary for eventual image reconstruction. This work presents a CMOS ASIC design for signal reducing readout electronics in support of an 8×8 silicon photomultiplier array. The row/column/diagonal summation circuit significantly reduces the number of required channels, reducing the cost of subsequent digitizing electronics. Current amplifiers are used with a single input from each SiPM cathode. This approach helps to reduce the detector loading, while generating all the necessary row, column and diagonal addressing information. In addition, the single current amplifier used in our Pulse-Positioning architecture facilitates the extraction of pulse timing information. Other components under design at present include a current-mode comparator which enables threshold detection for dark noise current reduction, a transimpedance amplifier and a variable output impedance I/O driver which adapts to a wide range of loading conditions between the ASIC and lines with the off-chip Analog-to-Digital Converters (ADCs).

Highly-Integrated CMOS Interface Circuits for SiPM-Based PET Imaging Systems

PubMed Central

Dey, Samrat; Lewellen, Thomas K.; Miyaoka, Robert S.; Rudell, Jacques C.

2013-01-01

Recent developments in the area of Positron Emission Tomography (PET) detectors using Silicon Photomultipliers (SiPMs) have demonstrated the feasibility of higher resolution PET scanners due to a significant reduction in the detector form factor. The increased detector density requires a proportionally larger number of channels to interface the SiPM array with the backend digital signal processing necessary for eventual image reconstruction. This work presents a CMOS ASIC design for signal reducing readout electronics in support of an 8×8 silicon photomultiplier array. The row/column/diagonal summation circuit significantly reduces the number of required channels, reducing the cost of subsequent digitizing electronics. Current amplifiers are used with a single input from each SiPM cathode. This approach helps to reduce the detector loading, while generating all the necessary row, column and diagonal addressing information. In addition, the single current amplifier used in our Pulse-Positioning architecture facilitates the extraction of pulse timing information. Other components under design at present include a current-mode comparator which enables threshold detection for dark noise current reduction, a transimpedance amplifier and a variable output impedance I/O driver which adapts to a wide range of loading conditions between the ASIC and lines with the off-chip Analog-to-Digital Converters (ADCs). PMID:24301987

Virus movement in soil columns flooded with secondary sewage effluent.

PubMed Central

Lance, J C; Gerba, C P; Melnick, J L

1976-01-01

Secondary sewage effluent containing about 3 X 10(4) plaque-forming units of polio virus type 1 (LSc) per ml was passed through columns 250 cm in length packed with calcareous sand from an area in the Salt River bed used for ground-water recharge of secondary sewage effluent. Viruses were not detected in 1-ml samples extracted from the columns below the 160-cm level. However, viruses were detected in 5 of 43 100-ml samples of the column drainage water. Most of the viruses were adsorbed in the top 5 cm of soil. Virus removal was not affected by the infiltration rate, which varied between 15 and 55 cm/day. Flooding a column continuosly for 27 days with the sewage water virus mixture did not saturate the top few centimeters of soil with viruses and did not seem to affect virus movement. Flooding with deionized water caused virus desorption from the soil and increased their movement through the columns. Adding CaCl2 to the deionized water prevented most of the virus desorption. Adding a pulse of deionized water followed by sewage water started a virus front moving through the columns, but the viruses were readsorbed and none was detected in outflow samples. Drying the soil for 1 day between applying the virus and flooding with deionized water greatly reduced desorption, and drying for 5 days prevented desorption. Large reductions (99.99% or more) of virus would be expected after passage of secondary sewage effluent through 250 cm of the calcareous sand similar to that used in our laboratory columns unless heavy rains fell within 1 day after the application of sewage stopped. Such virus movement could be minimized by the proper management of flooding and drying cycles. PMID:185960

Extreme degree of ionization in homogenous micro-capillary plasma columns heated by ultrafast current pulses.

PubMed

Avaria, G; Grisham, M; Li, J; Tomasel, F G; Shlyaptsev, V N; Busquet, M; Woolston, M; Rocca, J J

2015-03-06

Homogeneous plasma columns with ionization levels typical of megaampere discharges are created by rapidly heating gas-filled 520-μm-diameter channels with nanosecond rise time current pulses of 40 kA. Current densities of up to 0.3  GA cm^{-2} greatly increase Joule heating with respect to conventional capillary discharge Z pinches, reaching unprecedented degrees of ionization for a high-Z plasma column heated by a current pulse of remarkably low amplitude. Dense xenon plasmas are ionized to Xe^{28+}, while xenon impurities in hydrogen discharges reach Xe^{30+}. The unique characteristics of these hot, ∼300:1 length-to-diameter aspect ratio plasmas allow the observation of unexpected spectroscopic phenomena. Axial spectra show the unusual dominance of the intercombination line over the resonance line of He-like Al by nearly an order of magnitude, caused by differences in opacities in the axial and radial directions. These plasma columns could enable the development of sub-10-nm x-ray lasers.

Low-energy route for alcohol/gasohol recovery from fermentor beer. Final report

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

Mix, T.W.

1982-03-01

The production of gasohol directly from fermentor beer and gasoline is feasible and will enable a major reduction in the energy requirements for gasohol production. The fermentor beer is first enriched in a beer still to a 69 mol % ethanol, 31 mol % water product which is then dehydrated by extractive distillation with gasoline as the extractive agent. Gasohol is produced directly. In one version of the process, a heavy cut of gasoline, presumed available at a refinery before blending in of light components, is used as the extractive agent. The enriching column overhead vapors are used to reboilmore » the extractive distillation and steam stripping columns and to contribute to the preheating of the fermentor beer feed. Light components are blended into the heavy cut-ethanol bottom product from the extractive distillation column to form the desired gasohol. Energy requirements, including feed preheat, are 11,000 Btu per gallon of ethanol in the product gasohol. One hundred and fifty pound steam is required. In a second version, full range gasoline is used as the extractive agent. The enriching column overhead vapors are again used to reboil the extractive distillation and steam stripping columns and to contribute to the preheating of the fermentor beer feed. Light gasoline components recovered from the decanter following the overhead condenser of the extractive distillation column are blended in with the gasoline-ethanol product leaving the bottom of the extractive distillation column to form the desired gasohol. Energy requirements in this case are 13,000 Btu/gallon of ethanol in the product gasohol. In both of the above cases it is energy-conservative and desirable from a process standpoint to feed the enriched alcohol to the extractive distillation column as a liquid rather than as a vapor.« less

Laser ablation and column formation in silicon under oxygen-rich atmospheres

NASA Astrophysics Data System (ADS)

Pedraza, A. J.; Fowlkes, J. D.; Lowndes, D. H.

2000-11-01

The microstructure formed at the surface of silicon by cumulative pulsed-laser irradiation in oxygen-rich atmospheres consists of an array of microcolumns surrounded by microcanyons and microholes. Formation of SiOx at the exposed surface of silicon is most likely responsible for the occurrence of etching/ablation that causes the continuous deepening of canyons and holes. The growth mechanism of columns that is supported by the experimental evidence presented here is a process in which the columns are fed at their tips by the silicon-rich ablation plasma produced during pulsed-laser irradiation.

Volcanic eruption volume flux estimations from very long period infrasound signals

NASA Astrophysics Data System (ADS)

Yamada, Taishi; Aoyama, Hiroshi; Nishimura, Takeshi; Iguchi, Masato; Hendrasto, Muhamad

2017-01-01

We examine very long period infrasonic signals accompanying volcanic eruptions near active vents at Lokon-Empung volcano in Indonesia, Aso, Kuchinoerabujima, and Kirishima volcanoes in Japan. The excitation of the very long period pulse is associated with an explosion, the emerging of an eruption column, and a pyroclastic density current. We model the excitation of the infrasound pulse, assuming a monopole source, to quantify the volume flux and cumulative volume of erupting material. The infrasound-derived volume flux and cumulative volume can be less than half of the video-derived results. A largely positive correlation can be seen between the infrasound-derived volume flux and the maximum eruption column height. Therefore, our result suggests that the analysis of very long period volcanic infrasound pulses can be helpful in estimating the maximum eruption column height.

Space-based active optical remote sensing of carbon dioxide column using high-energy two-micron pulsed ipda lidar

NASA Astrophysics Data System (ADS)

Singh, Upendra N.; Refaat, Tamer F.; Ismail, Syed; Petros, Mulugeta; Davis, Kenneth J.; Kawa, Stephan R.; Menzies, Robert T.

2018-04-01

Modeling of a space-based high-energy 2-μm triple-pulse Integrated Path Differential Absorption (IPDA) lidar was conducted to demonstrate carbon dioxide (CO2) measurement capability and to evaluate random and systematic errors. A high pulse energy laser and an advanced MCT e-APD detector were incorporated in this model. Projected performance shows 0.5 ppm precision and 0.3 ppm bias in low-tropospheric column CO2 mixing ratio measurements from space for 10 second signal averaging over Railroad Valley (RRV) reference surface.

Airborne Double Pulsed 2-Micron IPDA Lidar for Atmospheric CO2 Measurement

NASA Technical Reports Server (NTRS)

Yu, Jirong; Petros, Mulugeta; Refaat, Tamer; Singh, Upendra

2015-01-01

We have developed an airborne 2-micron Integrated Path Differential Absorption (IPDA) lidar for atmospheric CO2 measurements. The double pulsed, high pulse energy lidar instrument can provide high-precision CO2 column density measurements.

Double-pulse THz radiation bursts from laser-plasma acceleration

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

Bosch, R. A.

2006-11-15

A model is presented for coherent THz radiation produced when an electron bunch undergoes laser-plasma acceleration and then exits axially from a plasma column. Radiation produced when the bunch is accelerated is superimposed with transition radiation from the bunch exiting the plasma. Computations give a double-pulse burst of radiation comparable to recent observations. The duration of each pulse very nearly equals the electron bunch length, while the time separation between pulses is proportional to the distance between the points where the bunch is accelerated and where it exits the plasma. The relative magnitude of the two pulses depends upon bymore » the radius of the plasma column. Thus, the radiation bursts may be useful in diagnosing the electron bunch length, the location of the bunch's acceleration, and the plasma radius.« less

PULSE COLUMN

DOEpatents

Grimmett, E.S.

1964-01-01

This patent covers a continuous countercurrent liquidsolids contactor column having a number of contactor states each comprising a perforated plate, a layer of balls, and a downcomer tube; a liquid-pulsing piston; and a solids discharger formed of a conical section at the bottom of the column, and a tubular extension on the lowest downcomer terminating in the conical section. Between the conical section and the downcomer extension is formed a small annular opening, through which solids fall coming through the perforated plate of the lowest contactor stage. This annular opening is small enough that the pressure drop thereacross is greater than the pressure drop upward through the lowest contactor stage. (AEC)

Simulation of multi-pulse coaxial helicity injection in the Sustained Spheromak Physics Experiment

NASA Astrophysics Data System (ADS)

O'Bryan, J. B.; Romero-Talamás, C. A.; Woodruff, S.

2018-03-01

Nonlinear, numerical computation with the NIMROD code is used to explore magnetic self-organization during multi-pulse coaxial helicity injection in the Sustained Spheromak Physics eXperiment. We describe multiple distinct phases of spheromak evolution, starting from vacuum magnetic fields and the formation of the initial magnetic flux bubble through multiple refluxing pulses and the eventual onset of the column mode instability. Experimental and computational magnetic diagnostics agree on the onset of the column mode instability, which first occurs during the second refluxing pulse of the simulated discharge. Our computations also reproduce the injector voltage traces, despite only specifying the injector current and not explicitly modeling the external capacitor bank circuit. The computations demonstrate that global magnetic evolution is fairly robust to different transport models and, therefore, that a single fluid-temperature model is sufficient for a broader, qualitative assessment of spheromak performance. Although discharges with similar traces of normalized injector current produce similar global spheromak evolution, details of the current distribution during the column mode instability impact the relative degree of poloidal flux amplification and magnetic helicity content.

TNT transport and fate in contaminated soil

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

Comfort, S.D.; Shea, P.J.; Hundal, L.S.

1995-11-01

Past disposal practices at munitions production plants have contaminated terrestrial and aquatk ecosystems with 2,4,6-trinitrotoluene (TNT). We determined TNT transport, degradation, and long-term sorption characteristics in soil. Transport experiments were conducted with repacked, unsaturated soil columns containing uncontaminated soil or layers of contaminated and uncontaminated soil. Uncontaminated soil columns received multiple pore volumes (22-50) of a TNT-{sup 3}H{sub 2}O pulse, containing 70 or 6.3 mg TNT L{sup -1} at a constant pore water velocity. TNT breakthrough curves (BTCs) never reached initial solute pulse concentrations. Apex concentrations (C/C{sub o}) were between 0.6 and 0.8 for an initial pulse of 70 mgmore » TNT L{sup -1} and 0.2 to 0.3 for the 6.3 mg TNT L{sup -1} pulse. Earlier TNT breakthrough was observed at the higher pulse concentration. This mobility difference was predicted from the nonlinear adsorption isotherm determined for TNT sorption. In all experiments, a significant fraction of added TNT was recovered as amino degradates of TNT. Mass balance estimates indicated 81% of the added TNT was recovered (as TNT and amino degradates) from columns receiving the 70 mg TNT L{sup -1} pulse compared to 35% from columns receiving the 6.3 mg TNT L{sup -1} pulse. Most of the unaccountable TNT was hypothesized to be unextractable. This was supported by a 168-d sorption experiment, which found that within 14d, 80% of {sup 14}C activity (added as {sup 14}C-TNT) was adsorbed and roughly 40% unextractable. Our observations illustrate that TNT sorption and degradation are concentration-dependent and the assumptions of linear adsorption and adsorption-desorption singularity commonly used in transport modeling, may not be valid for predicting TNT transport in munitions-contaminated soils. 29 refs., 6 figs., 7 tabs.« less

Column-to-column packing variation of disposable pre-packed columns for protein chromatography.

PubMed

Schweiger, Susanne; Hinterberger, Stephan; Jungbauer, Alois

2017-12-08

In the biopharmaceutical industry, pre-packed columns are the standard for process development, but they must be qualified before use in experimental studies to confirm the required performance of the packed bed. Column qualification is commonly done by pulse response experiments and depends highly on the experimental testing conditions. Additionally, the peak analysis method, the variation in the 3D packing structure of the bed, and the measurement precision of the workstation influence the outcome of qualification runs. While a full body of literature on these factors is available for HPLC columns, no comparable studies exist for preparative columns for protein chromatography. We quantified the influence of these parameters for commercially available pre-packed and self-packed columns of disposable and non-disposable design. Pulse response experiments were performed on 105 preparative chromatography columns with volumes of 0.2-20ml. The analyte acetone was studied at six different superficial velocities (30, 60, 100, 150, 250 and 500cm/h). The column-to-column packing variation between disposable pre-packed columns of different diameter-length combinations varied by 10-15%, which was acceptable for the intended use. The column-to-column variation cannot be explained by the packing density, but is interpreted as a difference in particle arrangement in the column. Since it was possible to determine differences in the column-to-column performance, we concluded that the columns were well-packed. The measurement precision of the chromatography workstation was independent of the column volume and was in a range of±0.01ml for the first peak moment and±0.007 ml 2 for the second moment. The measurement precision must be considered for small columns in the range of 2ml or less. The efficiency of disposable pre-packed columns was equal or better than that of self-packed columns. Copyright © 2017 The Author(s). Published by Elsevier B.V. All rights reserved.

Liquid chromatographic extraction medium

DOEpatents

Horwitz, E. Philip; Dietz, Mark L.

1994-01-01

A method and apparatus for extracting strontium and technetium values from biological, industrial and environmental sample solutions using a chromatographic column is described. An extractant medium for the column is prepared by generating a solution of a diluent containing a Crown ether and dispersing the solution on a resin substrate material. The sample solution is highly acidic and is introduced directed to the chromatographic column and strontium or technetium is eluted using deionized water.

Nonmonotonic radial distribution of excited atoms in a positive column of pulsed direct currect discharges in helium

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

Barnat, E. V.; Kolobov, V. I.

2013-01-21

Nonmonotonic radial distributions of excited helium atoms have been experimentally observed in a positive column of pulsed helium discharges using planar laser induced fluorescence. Computational analysis of the discharge dynamics with a fluid plasma model confirms the experimental observations over a range of pressures and currents. The observed effect is attributed to the peculiarities of electron population-depopulation of the excited states during the 'dynamic discharge' conditions with strong modulations of the electric field maintaining the plasma.

Influence of soil moisture on sunflower oil extraction of polycyclic aromatic hydrocarbons from a manufactured gas plant soil.

PubMed

Gong, Zongqiang; Wilke, B-M; Alef, Kassem; Li, Peijun

2005-05-01

The influence of soil moisture on efficiency of sunflower oil extraction of polycyclic aromatic hydrocarbons (PAHs) from contaminated soil was investigated. The PAH-contaminated soil was collected from a manufactured gas plant (MGP) site in Berlin, Germany. Half of the soil was air-dried, and the other half was kept as field-moist soil. Batch experiments were performed using air-dried and field-moist soils, and sunflower oil was used as extractant at oil/soil ratios of 2:1 and 1:1 (v/m). The experimental data were fitted to a first-order empirical model to describe mass-transfer profiles of the PAHs. Column extraction experiments were also conducted. Field-moist and air-dried soils in the column were extracted using sunflower oil at an oil/soil ratio of 2:1. In the batch experiments, PAHs were more rapidly extracted from air-dried soil than from field-moist soil. Removal rate of total PAH increased 23% at oil/soil ratio of 1:1 and 15.5% at oil/soil ratio of 2:1 after the soil was air dried. The most favorable conditions for batch extraction were air-dried soil, with an oil/soil ratio of 2:1. In the column experiments, the removal rate of total PAH from air-dried soil was 30.7% higher than that from field-moist soil. For field-moist soil, extraction efficiencies of the batch extraction (67.2% and 81.5%) were better than that for column extraction (65.6%). However, this difference between the two methods became less significant for the air-dried soil, with a total removal rate of 96.3% for column extraction and 90.2% and 97% for batch extractions. A mass-balance test was carried out for analytical quality assurance. The results of both batch and column experiments indicated that drying the soil increased efficiency of extraction of PAHs from the MGP soil.

40 CFR 141.40 - Monitoring requirements for unregulated contaminants.

Code of Federal Regulations, 2011 CFR

2011-07-01

... monitoring to be completed Reserved i Reserved i Reserved i Reserved i Reserved i Reserved i Column headings... Pesticides and Flame Retardants in Drinking Water by Solid Phase Extraction and Capillary Column Gas... Water by Solid Phase Extraction and Capillary Column Gas Chromatography/Mass Spectrometry (GC/MS...

Liquid chromatographic extraction medium

DOEpatents

Horwitz, E.P.; Dietz, M.L.

1994-09-13

A method and apparatus are disclosed for extracting strontium and technetium values from biological, industrial and environmental sample solutions using a chromatographic column. An extractant medium for the column is prepared by generating a solution of a diluent containing a Crown ether and dispersing the solution on a resin substrate material. The sample solution is highly acidic and is introduced directed to the chromatographic column and strontium or technetium is eluted using deionized water. 1 fig.

a Compact, Rf-Driven Pulsed Ion Source for Intense Neutron Generation

NASA Astrophysics Data System (ADS)

Perkins, L. T.; Celata, C. M.; Lee, Y.; Leung, K. N.; Picard, D. S.; Vilaithong, R.; Williams, M. D.; Wutte, D.

1997-05-01

Lawrence Berkeley National Laboratory is currently developing a compact, sealed-accelerator-tube neutron generator capable of producing a neutron flux in the range of 109 to 1010 D-T neutrons per second. The ion source, a miniaturized variation of earlier 2 MHz radio-frequency (rf)-driven multicusp ion sources, is designed to fit within a #197# 5 cm diameter borehole. Typical operating parameters include repetition rates up to 100 pps, with pulse widths between 10 and 80 us and source pressures as low as #197# 5 mTorr. In this configuration, peak extractable hydrogen current exceeding 35 mA from a 2 mm diameter aperture together with H1+ yields over 94% have been achieved. The required rf impedance matching network has been miniaturized to #197# 5 cm diameter. The accelerator column is a triode design using the IGUN ion optics codes and allows for electron suppression. Results from the testing of the integrated matching network-ion source-accelerator system will be presented.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of pesticides in water by C-18 solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion monitoring

USGS Publications Warehouse

Zaugg, Steven D.; Sandstrom, Mark W.; Smith, Steven G.; Fehlberg, Kevin M.

1995-01-01

A method for the isolation of 41 pesticides and pesticide metabolites in natural-water samples using C-18 solid-phase extraction and determination by capillary-column gas chromatography/mass spectrometry with selected-ion monitoring is described. Water samples are filtered to remove suspended particulate matter and then are pumped through disposable solid-phase extraction columns containing octadecyl-bonded porous silica to extract the pesticides. The columns are dried using carbon dioxide or nitrogen gas, and adsorbed pesticides are removed from the columns by elution with 3.0 milliliters of hexane-isopropanol (3:1). Extracted pesticides are determined by capillary- column gas chromatography/mass spectrometry with selected-ion monitoring of three characteristic ions. The upper concentration limit is 4 micrograms per liter (g/L) for most pesticides, with the exception of widely used corn herbicides--atrazine, alachlor, cyanazine, and metolachlor--which have upper concentration limits of 20 g/L. Single- operator method detection limits in reagent-water samples range from 0.001 to 0.018 g/L. Average short-term single-operator precision in reagent- water samples is 7 percent at the 0.1- and 1.0-g/L levels and 8 percent at the 0.01-g/L level. Mean recoveries in reagent-water samples are 73 percent at the 0.1- and 1.0-g/L levels and 83 percent at the 0.01-g/L level. The estimated holding time for pesticides after extraction on the solid-phase extraction columns was 7 days. An optional on-site extraction procedure allows for samples to be collected and processed at remote sites where it is difficult to ship samples to the laboratory within the recommended pre-extraction holding time.

Effects of Gravity on Cocurrent Two-Phase Gas-Liquid Flows Through Packed Columns

NASA Technical Reports Server (NTRS)

Motil, Brian J.; Balakotaiah, Vemuri; Kamotani, Yasuhiro

2001-01-01

This work presents the experimental results of research on the influence of gravity on flow pattern transitions, pressure drop and flow characteristics for cocurrent gas-liquid two-phase flow through packed columns. The flow pattern transition data indicates that the pulse flow regime exists over a wider range of gas and liquid flow rates under reduced gravity conditions compared to normal gravity cocurrent down-flow. This is illustrated by comparing the flow regime transitions found in reduced gravity with the transitions predicted by Talmor. Next, the effect of gravity on the total pressure drop in a packed column is shown to depend on the flow regime. The difference is roughly equivalent to the liquid static head for bubbly flow but begins to decrease at the onset of pulse flow. As the spray flow regime is approached by increasing the gas to liquid ratio, the effect of gravity on pressure drop becomes negligible. Finally, gravity tends to suppress the amplitude of each pressure pulse. An example of this phenomenon is presented.

Method for liquid chromatographic extraction of strontium from acid solutions

DOEpatents

Horwitz, E. Philip; Dietz, Mark L.

1992-01-01

A method and apparatus for extracting strontium and technetium values from biological, industrial and environmental sample solutions using a chromatographic column is described. An extractant medium for the column is prepared by generating a solution of a diluent containing a Crown ether and dispersing the solution on a resin substrate material. The sample solution is highly acidic and is introduced directed to the chromatographic column and strontium or technetium is eluted using deionized water.

10 CFR Appendix J to Part 110 - Illustrative List of Uranium Conversion Plant Equipment and Plutonium Conversion Plant Equipment...

Code of Federal Regulations, 2010 CFR

2010-01-01

... reactors, flame tower reactors, liquid centrifuges, distillation columns and liquid-liquid extraction... to UF6 is performed by exothermic reaction with fluorine in a tower reactor. UF6 is condensed from..., flame tower reactors, liquid centrifuges, distillation columns and liquid-liquid extraction columns. Hot...

Selective Permeation and Organic Extraction of Recombinant Green Fluorescent Protein (gfpuv) from Escherichia coli

PubMed Central

2002-01-01

Background Transformed cells of Escherichia coli DH5-α with pGFPuv, induced by IPTG (isopropyl-β-d-thiogalactopyranoside), express the green fluorescent protein (gfpuv) during growth phases. E. coli subjected to the combination of selective permeation by freezing/thawing/sonication cycles followed by the three-phase partitioning extraction (TPP) method were compared to the direct application of TPP to the same culture of E. coli on releasing gfpuv from the over-expressing cells. Material and Methods Cultures (37°C/100 rpm/ 24 h; μ = 0.99 h-1 - 1.10 h-1) of transformed (pGFP) Escherichia coli DH5-α, expressing the green fluorescent protein (gfpuv, absorbance at 394 nm and emission at 509 nm) were sonicated in successive intervals of sonication (25 vibrations/pulse) to determine the maximum amount of gfpuv released from the cells. For selective permeation, the transformed previously frozen (-75°C) cells were subjected to three freeze/thaw (-20°C/ 0.83°C/min) cycles interlaid by sonication (3 pulses/ 6 seconds/ 25 vibrations). The intracellular permeate with gfpuv in extraction buffer (TE) solution (25 mM Tris-HCl, pH 8.0, 1 mM β-mercaptoethanol β-ME, 0.1 mM PMSF) was subjected to the three-phase partitioning (TPP) method with t-butanol and 1.6 M ammonium sulfate. Sonication efficiency was verified on the application to the cells previously treated by the TPP method. The intra-cell releases were mixed and eluted through methyl HIC column with a buffer solution (10 mM Tris-HCl, 10 mM EDTA, pH 8.0). Results The sonication maximum released amount obtained from the cells was 327.67 μg gfpuv/mL (20.73 μg gfpuv/mg total proteins – BSA), after 9 min of treatment. Through the selective permeation by three repeated freezing/thawing/sonication cycles applied to the cells, a close content of 241.19 μg gfpuv/mL (29.74 μg gfpuv/mg BSA) was obtained. The specific mass range of gfpuv released from the same cultures, by the three-phase partitioning (TPP) method, in relation to total proteins, was higher, between 107.28 μg/mg and 135.10 μg/mg. Conclusions The selective permeation of gfpuv by freezing/thawing/sonication followed by TPP separation method was equivalent to the amount of gfpuv extracted from the cells directly by TPP; although selective permeation extracts showed better elution through the HIC column. PMID:11972900

Event sequence detector

NASA Technical Reports Server (NTRS)

Hanna, M. F. (Inventor)

1973-01-01

An event sequence detector is described with input units, each associated with a row of bistable elements arranged in an array of rows and columns. The detector also includes a shift register which is responsive to clock pulses from any of the units to sequentially provide signals on its output lines each of which is connected to the bistable elements in a corresponding column. When the event-indicating signal is received by an input unit it provides a clock pulse to the shift register to provide the signal on one of its output lines. The input unit also enables all its bistable elements so that the particular element in the column supplied with the signal from the register is driven to an event-indicating state.

Repetitive Regeneration of Media #1 in a Dynamic Column Extraction using Brine #1

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

Gary Garland

This data is from a regeneration study from a dynamic column extraction experiment where we ran a solution of REE's through a column of media #1 then stripped the REE's off the media using 2M HNO3 solution. We then re-equilibrated the media and repeated the process of running a REE solution through the column and stripping the REE's off the media and comparing the two runs.

Study on the extraction and purification of glycoprotein from the yellow seahorse, Hippocampus kuda Bleeker

PubMed Central

Su, Yuting; Xu, Yongjian

2015-01-01

The optimum parameters of extraction for glycoprotein from seahorse were examined and determined by Box-Behnken combined with ultrasonic extraction technology. Column chromatography of glycoprotein was used for further purification. The optimal extraction conditions of seahorse glycoprotein were extracting time 4.3 h, salt concentration 0.08 mol/L, extracting temperature 73°C, raw material, and water ratio 1:6. At the optimal conditions, the yield of saccharide reached to 1.123%, and the yield of protein reached to 5.898%. For purifying the crude glycoprotein, the stage renounces of DEAE-52 column chromatography were done, respectively, with 0.05, 0.1, 0.5 mol/L NaHCO3 solution, and further purification was done with Sephadex G-100 column chromatography. Finally, two pieces of seahorse glycoprotein were obtained by the column chromatography, that is, HG-11 and HG-21. The saccharide content was 56.7975% and 39.479%, the protein content was 30.5475% and 51.747%, respectively. PMID:26288722

Ultra-short ion and neutron pulse production

DOEpatents

Leung, Ka-Ngo; Barletta, William A.; Kwan, Joe W.

2006-01-10

An ion source has an extraction system configured to produce ultra-short ion pulses, i.e. pulses with pulse width of about 1 .mu.s or less, and a neutron source based on the ion source produces correspondingly ultra-short neutron pulses. To form a neutron source, a neutron generating target is positioned to receive an accelerated extracted ion beam from the ion source. To produce the ultra-short ion or neutron pulses, the apertures in the extraction system of the ion source are suitably sized to prevent ion leakage, the electrodes are suitably spaced, and the extraction voltage is controlled. The ion beam current leaving the source is regulated by applying ultra-short voltage pulses of a suitable voltage on the extraction electrode.

In vitro investigations of propulsion during laser lithotripsy using video tracking.

PubMed

Eisel, Maximilian; Ströbl, Stephan; Pongratz, Thomas; Strittmatter, Frank; Sroka, Ronald

2018-04-01

Ureteroscopic laser lithotripsy is an important and widely used method for destroying ureter stones. It represents an alternative to ultrasonic and pneumatic lithotripsy techniques. Although these techniques have been thoroughly investigated, the influence of some physical parameters that may be relevant to further improve the treatment results is not fully understood. One crucial topic is the propulsive stone movement induced by the applied laser pulses. To simplify and speed up the optimization of laser parameters in this regard, a video tracking method was developed in connection with a vertical column setup that allows recording and subsequently analyzing the propulsive stone movement in dependence of different laser parameters in a particularly convenient and fast manner. Pulsed laser light was applied from below to a cubic BegoStone phantom loosely guided within a vertical column setup. The video tracking method uses an algorithm to determine the vertical stone position in each frame of the recorded scene. The time-dependence of the vertical stone position is characterized by an irregular series of peaks. By analyzing the slopes of the peaks in this signal it was possible to determine the mean upward stone velocity for a whole pulse train and to compare it for different laser settings. For a proof of principle of the video tracking method, a specific pulse energy setting (1 J/pulse) was used in combination with three different pulse durations: short pulse (0.3 ms), medium pulse (0.6 ms), and long pulse (1.0 ms). The three pulse durations were compared in terms of their influence on the propulsive stone movement in terms of upward velocity. Furthermore, the propulsions induced by two different pulse energy settings (0.8 J/pulse and 1.2 J/pulse) for a fixed pulse duration (0.3 ms) were compared. A pulse repetition rate of 10 Hz was chosen for all experiments, and for each laser setting, the experiment was repeated on 15 different freshly prepared stones. The latter set of experiments was compared with the results of previous propulsion measurements performed with a pendulum setup. For a fixed pulse energy (1 J/pulse), the mean upward propulsion velocity increased (from 120.0 to 154.9 mm · s -1 ) with decreasing pulse duration. For fixed pulse duration (0.3 ms), the mean upward propulsion velocity increased (from 91.9 to 123.3 mm · s -1 ) with increasing pulse energy (0.8 J/pulse and 1.2 J/pulse). The latter result corresponds roughly to the one obtained with the pendulum setup (increase from 61 to 105 mm · s -1 ). While the mean propulsion velocities for the two different pulse energies were found to differ significantly (P < 0.001) for the two experimental and analysis methods, the standard deviations of the measured mean propulsion velocities were considerably smaller in case of the vertical column method with video tracking (12% and 15% for n = 15 freshly prepared stones) than in case of the pendulum method (26% and 41% for n = 50 freshly prepared stones), in spite of the considerably smaller number of experiment repetitions ("sample size") in the first case. The proposed vertical column method with video tracking appears advantageous compared to the pendulum method in terms of the statistical significance of the obtained results. This may partly be understood by the fact that the entire motion of the stones contributes to the data analysis, rather than just their maximum distance from the initial position. The key difference is, however, that the pendulum method involves only one single laser pulse in each experiment run, which renders this method rather tedious to perform. Furthermore, the video tracking method appears much better suited to model a clinical lithotripsy intervention that utilizes longer series of laser pulses at higher repetition rates. The proposed video tracking method can conveniently and quickly deliver results for a large number of laser pulses that can easily be averaged. An optimization of laser settings to achieve minimal propulsive stone movement should thus be more easily feasible with the video tracking method in connection with the vertical column setup. Lasers Surg. Med. 50:333-339, 2018. © 2017 Wiley Periodicals, Inc. © 2017 Wiley Periodicals, Inc.

Quick, easy, cheap, effective, rugged, and safe sample preparation approach for pesticide residue analysis using traditional detectors in chromatography: A review.

PubMed

Rahman, Md Musfiqur; Abd El-Aty, A M; Kim, Sung-Woo; Shin, Sung Chul; Shin, Ho-Chul; Shim, Jae-Han

2017-01-01

In pesticide residue analysis, relatively low-sensitivity traditional detectors, such as UV, diode array, electron-capture, flame photometric, and nitrogen-phosphorus detectors, have been used following classical sample preparation (liquid-liquid extraction and open glass column cleanup); however, the extraction method is laborious, time-consuming, and requires large volumes of toxic organic solvents. A quick, easy, cheap, effective, rugged, and safe method was introduced in 2003 and coupled with selective and sensitive mass detectors to overcome the aforementioned drawbacks. Compared to traditional detectors, mass spectrometers are still far more expensive and not available in most modestly equipped laboratories, owing to maintenance and cost-related issues. Even available, traditional detectors are still being used for analysis of residues in agricultural commodities. It is widely known that the quick, easy, cheap, effective, rugged, and safe method is incompatible with conventional detectors owing to matrix complexity and low sensitivity. Therefore, modifications using column/cartridge-based solid-phase extraction instead of dispersive solid-phase extraction for cleanup have been applied in most cases to compensate and enable the adaptation of the extraction method to conventional detectors. In gas chromatography, the matrix enhancement effect of some analytes has been observed, which lowers the limit of detection and, therefore, enables gas chromatography to be compatible with the quick, easy, cheap, effective, rugged, and safe extraction method. For liquid chromatography with a UV detector, a combination of column/cartridge-based solid-phase extraction and dispersive solid-phase extraction was found to reduce the matrix interference and increase the sensitivity. A suitable double-layer column/cartridge-based solid-phase extraction might be the perfect solution, instead of a time-consuming combination of column/cartridge-based solid-phase extraction and dispersive solid-phase extraction. Therefore, replacing dispersive solid-phase extraction with column/cartridge-based solid-phase extraction in the cleanup step can make the quick, easy, cheap, effective, rugged, and safe extraction method compatible with traditional detectors for more sensitive, effective, and green analysis. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

10 CFR Appendix J to Part 110 - Illustrative List of Uranium Conversion Plant Equipment and Plutonium Conversion Plant Equipment...

Code of Federal Regulations, 2011 CFR

2011-01-01

... reactors, flame tower reactors, liquid centrifuges, distillation columns and liquid-liquid extraction... UF4 to UF6 is performed by exothermic reaction with fluorine in a tower reactor. UF6 is condensed from..., flame tower reactors, liquid centrifuges, distillation columns and liquid-liquid extraction columns. Hot...

Airborne Measurements of Atmospheric Methane Column Abundance Made Using a Pulsed IPDA Lidar

NASA Technical Reports Server (NTRS)

Riris, Haris; Numata, Kenji; Li, Steve; Wu, Stewart; Ramanathan, Anamd; Dawsey, Martha; Mao, Jianping; Kawa, Randolph; Abshire, James B.

2012-01-01

We report airborne measurements of the column abundance of atmospheric methane made over an altitude range of 3-11 km using a direct detection IPDA lidar with a pulsed laser emitting at 1651 nm. The laser transmitter was a tunable, seeded optical parametric amplifier (OPA) pumped by a Nd:YAG laser and the receiver used a photomultiplier detector and photon counting electronics. The results follow the expected changes with aircraft altitude and the measured line shapes and optical depths show good agreement with theoretical calculations.

Computer Simulation of Global Profiles of Carbon Dioxide Using a Pulsed, 2-Micron, Coherent-Detection, Column-Content DIAL System

NASA Technical Reports Server (NTRS)

Kavaya, Michael J.; Singh, Upendra N.; Koch, Grady J.; Yu, Jirong; Frehlich, Rod G.

2009-01-01

We present preliminary results of computer simulations of the error in measuring carbon dioxide mixing ratio profiles from earth orbit. The simulated sensor is a pulsed, 2-micron, coherent-detection lidar alternately operating on at least two wavelengths. The simulated geometry is a nadir viewing lidar measuring the column content signal. Atmospheric absorption is modeled using FASCODE3P software with the HITRAN 2004 absorption line data base. Lidar shot accumulation is employed up to the horizontal resolution limit. Horizontal resolutions of 50, 100, and 200 km are shown. Assuming a 400 km spacecraft orbit, the horizontal resolutions correspond to measurement times of about 7, 14, and 28 s. We simulate laser pulse-pair repetition frequencies from 1 Hz to 100 kHz. The range of shot accumulation is 7 to 2.8 million pulse-pairs. The resultant error is shown as a function of horizontal resolution, laser pulse-pair repetition frequency, and laser pulse energy. The effect of different on and off pulse energies is explored. The results are compared to simulation results of others and to demonstrated 2-micron operating points at NASA Langley.

The setup of an extraction system coupled to a hydrogen isotopes distillation column

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

Zamfirache, M.; Bornea, A.; Stefanescu, I.

2008-07-15

Among the most difficult problems of cryogenic distillation one stands apart: the extraction of the heavy fraction. By an optimal design of the cycle scheme, this problem could be avoided. A 'worst case scenario' is usually occurring when the extracted fraction consists of one prevalent isotope such as hydrogen and small amounts of the other two hydrogen isotopes (deuterium and/or tritium). This situation is further complicated by two parameters of the distillation column: the extraction flow rate and the hold-up. The present work proposes the conceptual design of an extraction system associated to the cryogenic distillation column used in hydrogenmore » separation processes. During this process, the heavy fraction (DT, T{sub 2}) is separated, its concentration being the highest at the bottom of the distillation column. From this place the extraction of the gaseous phase can now begin. Being filled with adsorbent, the extraction system is used to temporarily store the heavy fraction. Also the extraction system provides samples for the gas Chromatograph. The research work is focused on the existent pilot plant for tritium and deuterium separation from our institute to validate the experiments carried out until now. (authors)« less

Application of EDTA decontamination on soils affected by mining activities and impact of treatment on the geochemical partition of metal contaminants.

PubMed

Xia, Wenbin; Gao, Hui; Wang, Xianhai; Zhou, Chunhua; Liu, Yunguo; Fan, Ting; Wang, Xin

2009-05-30

Two soil samples were collected at mining areas located in southern Hunan Province, China. EDTA extraction of Pb, Zn, Cu and Cd from these two tailing soils was studied using column leaching experiments. The redistributions of heavy metals (HMs) were determined using the modified BCR (Community Bureau of Reference) sequential extraction procedure, before and after EDTA extraction. The results indicated that EDTA was an effective extractant because of its strong chelating ability for various HMs. The proportions of Pb, Zn, Cu and Cd in the four fractions varied largely after EDTA extraction. The extraction efficiency of EDTA of the acid-extractable fraction (AEX) was significant in shallow soil column, while in deeper soil column, decrease of the extraction efficiency of reduced (RED), oxidizable (OX) and residual fractions (RES) was obtained, which was mainly due to the decrease of EDTA concentration.

Ultrasonic Fingerprint Sensor With Transmit Beamforming Based on a PMUT Array Bonded to CMOS Circuitry.

PubMed

Jiang, Xiaoyue; Tang, Hao-Yen; Lu, Yipeng; Ng, Eldwin J; Tsai, Julius M; Boser, Bernhard E; Horsley, David A

2017-09-01

In this paper, we present a single-chip 65 ×42 element ultrasonic pulse-echo fingerprint sensor with transmit (TX) beamforming based on piezoelectric micromachined ultrasonic transducers directly bonded to a CMOS readout application-specific integrated circuit (ASIC). The readout ASIC was realized in a standard 180-nm CMOS process with a 24-V high-voltage transistor option. Pulse-echo measurements are performed column-by-column in sequence using either one column or five columns to TX the ultrasonic pulse at 20 MHz. TX beamforming is used to focus the ultrasonic beam at the imaging plane where the finger is located, increasing the ultrasonic pressure and narrowing the 3-dB beamwidth to [Formula: see text], a factor of 6.4 narrower than nonbeamformed measurements. The surface of the sensor is coated with a poly-dimethylsiloxane (PDMS) layer to provide good acoustic impedance matching to skin. Scanning laser Doppler vibrometry of the PDMS surface was used to map the ultrasonic pressure field at the imaging surface, demonstrating the expected increase in pressure, and reduction in beamwidth. Imaging experiments were conducted using both PDMS phantoms and real fingerprints. The average image contrast is increased by a factor of 1.5 when beamforming is used.

On the radiation beaming of bright X-ray pulsars and constraints on neutron star mass-radius relation

NASA Astrophysics Data System (ADS)

Mushtukov, Alexander A.; Verhagen, Patrick A.; Tsygankov, Sergey S.; van der Klis, Michiel; Lutovinov, Alexander A.; Larchenkova, Tatiana I.

2018-03-01

The luminosity of accreting magnetized neutron stars can largely exceed the Eddington value due to appearance of accretion columns. The height of the columns can be comparable to the neutron star radius. The columns produce the X-rays detected by the observer directly and illuminate the stellar surface, which reprocesses the X-rays and causes additional component of the observed flux. The geometry of the column and the illuminated part of the surface determine the radiation beaming. Curved space-time affects the angular flux distribution. We construct a simple model of the beam patterns formed by direct and reflected flux from the column. We take into account the possibility of appearance of accretion columns, whose height is comparable to the neutron star radius. We argue that depending on the compactness of the star, the flux from the column can be either strongly amplified due to gravitational lensing, or significantly reduced due to column eclipse by the star. The eclipses of high accretion columns result in specific features in pulse profiles. Their detection can put constraints on the neutron star radius. We speculate that column eclipses are observed in X-ray pulsar V 0332+53, leading us to the conclusion of large neutron star radius in this system (˜15 km if M ˜ 1.4 M⊙). We point out that the beam pattern can be strongly affected by scattering in the accretion channel at high luminosity, which has to be taken into account in the models reproducing the pulse profiles.

Advances in High Energy Solid-State Pulsed 2-Micron Lidar Development for Ground and Airborne Wind, Water Vapor and CO2 Measurements

NASA Technical Reports Server (NTRS)

Singh, Upendra N.; Yu, Jirong; Petros, Mulugeta; Refaat, Tamer; Kavaya, Michael J.; Remus, Ruben

2015-01-01

NASA Langley Research Center has a long history of developing 2-micron lasers. From fundamental spectroscopy research, theoretical prediction of new materials, laser demonstration and engineering of lidar systems, it has been a very successful program spanning around two decades. Successful development of 2-micron lasers has led to development of a state-of-the-art compact lidar transceiver for a pulsed coherent Doppler lidar system for wind measurement with an unprecedented laser pulse energy of 250 millijoules in a rugged package. This high pulse energy is produced by a Ho:Tm:LuLiF laser with an optical amplifier. While the lidar is meant for use as an airborne instrument, ground-based tests were carried out to characterize performance of the lidar. Atmospheric measurements will be presented, showing the lidar's capability for wind measurement in the atmospheric boundary layer and free troposphere. Lidar wind measurements are compared to a balloon sonde, showing good agreement between the two sensors. Similar architecture has been used to develop a high energy, Ho:Tm:YLF double-pulsed 2-micron Integrated Differential Absorption Lidar (IPDA) instrument based on direct detection technique that provides atmospheric column CO2 measurements. This instrument has been successfully used to measure atmospheric CO2 column density initially from a ground mobile lidar trailer, and then it was integrated on B-200 plane and 20 hours of flight measurement were made from an altitude ranging 1500 meters to 8000 meters. These measurements were compared to in-situ measurements and National Oceanic and Atmospheric Administration (NOAA) airborne flask measurement to derive the dry mixing ratio of the column CO2 by reflecting the signal by various reflecting surfaces such as land, vegetation, ocean surface, snow and sand. The lidar measurements when compared showed a very agreement with in-situ and airborne flask measurement. NASA Langley Research Center is currently developing a triple-pulsed 2-micron Integrated Differential Absorption Lidar (IPDA) instrument for simultaneous measurement of water vapor and carbon-dioxide column density measurement from an air-borne platform. This presentation will give an overview of the 2 decades of 2-micron coherent and direction detection of laser/lidar development at NASA Langley Research Center and will present the ground and airborne wind and column CO2 measurement intercomparison with in-situ, balloon and flask measurements.

Separation of actinides using capillary extraction chromatography-inductively coupled plasma mass spectrometry.

PubMed

Peterson, Dominic S; Montoya, Velma M

2009-08-01

Trace levels of actinides have been separated on capillary extraction chromatography columns. Detection of the actinides was achieved using an inductively coupled plasma mass spectrometer, which was coupled with the extraction chromatography system. In this study, we compare 30-cm long, 4.6 mm i.d. columns to capillary columns (750 microm i.d.) with lengths from 30 cm up to 150 cm. The columns that were tested were packed with TRU resin. We were able to separate a mixture of five actinides ((232)Th, (238)U, (237)Np, (239)Pu, and (241)Am). This work has application to rapid bioassay as well as automated separations of actinide materials.

Cavity Optical Pulse Extraction: ultra-short pulse generation as seeded Hawking radiation.

PubMed

Eilenberger, Falk; Kabakova, Irina V; de Sterke, C Martijn; Eggleton, Benjamin J; Pertsch, Thomas

2013-01-01

We show that light trapped in an optical cavity can be extracted from that cavity in an ultrashort burst by means of a trigger pulse. We find a simple analytic description of this process and show that while the extracted pulse inherits its pulse length from that of the trigger pulse, its wavelength can be completely different. Cavity Optical Pulse Extraction is thus well suited for the development of ultrashort laser sources in new wavelength ranges. We discuss similarities between this process and the generation of Hawking radiation at the optical analogue of an event horizon with extremely high Hawking temperature. Our analytic predictions are confirmed by thorough numerical simulations.

Cavity Optical Pulse Extraction: ultra-short pulse generation as seeded Hawking radiation

PubMed Central

Eilenberger, Falk; Kabakova, Irina V.; de Sterke, C. Martijn; Eggleton, Benjamin J.; Pertsch, Thomas

2013-01-01

We show that light trapped in an optical cavity can be extracted from that cavity in an ultrashort burst by means of a trigger pulse. We find a simple analytic description of this process and show that while the extracted pulse inherits its pulse length from that of the trigger pulse, its wavelength can be completely different. Cavity Optical Pulse Extraction is thus well suited for the development of ultrashort laser sources in new wavelength ranges. We discuss similarities between this process and the generation of Hawking radiation at the optical analogue of an event horizon with extremely high Hawking temperature. Our analytic predictions are confirmed by thorough numerical simulations. PMID:24060831

Developing the Pulsed Fission-Fusion (PuFF) Engine

NASA Technical Reports Server (NTRS)

Adams, Robert B.; Cassibry, Jason; Bradley, David; Fabisinski, Leo; Statham, Geoffrey

2014-01-01

In September 2013 the NASA Innovative Advanced Concept (NIAC) organization awarded a phase I contract to the PuFF team. Our phase 1 proposal researched a pulsed fission-fusion propulsion system that compressed a target of deuterium (D) and tritium (T) as a mixture in a column, surrounded concentrically by Uranium. The target is surrounded by liquid lithium. A high power current would flow down the liquid lithium and the resulting Lorentz force would compress the column by roughly a factor of 10. The compressed column would reach criticality and a combination of fission and fusion reactions would occur. Our Phase I results, summarized herein, review our estimates of engine and vehicle performance, our work to date to model the fission-fusion reaction, and our initial efforts in experimental analysis.

Measurement of bromate in bread by liquid chromatography with post-column flow reactor detection.

PubMed

Himata, K; Noda, M; Ando, S; Yamada, Y

2000-01-01

This method is suitable for the determination of bromate residues in a variety of baked goods. The peer-verified method trial was performed on white bread, multigrain bread, and coffee cake spiked with known levels of potassium bromate. The analytical portion is extracted with deionized water to remove bromate from the bulk of the baked product. The aqueous extract is carried through a series of steps to remove co-extractives that would interfere with the liquid chromatography (LC) in the determinative step or hasten the deterioration of the LC column. The extract is filtered before passing it through a reversed-phase solid-phase extraction (SPE) column and a cation-exchange column in the silver form to remove lipids and chloride, respectively. Ultrafiltration is then used to remove proteins with molecular weights of >30,000 daltons. Finally, a cation-exchange column in the sodium form is used to remove silver ions from the extract. The determinative step uses LC with a reversed-phase column and an ion-pairing agent in the mobile phase. Detection is based on the post-column reaction of bromate with o-dianisidine to form an oxidation product that is quantitated spectrophotometrically at 450 nm. Overall agreement between the submitting and peer laboratories was quite good. For bromate levels of 10-52 ppb, overall mean recoveries were 76.9 and 78.8% for the submitting and peer laboratories, respectively. The standard deviations were higher for the results of the peer laboratory, probably because of the generally higher level of baseline noise present in the chromatograms. The results demonstrate that the method provides adequate accuracy with low-fat as well as high-fat foods. Bromate at levels as low as 5 ppb (ng/g) can be detected with the method.

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.

Online hyphenation of extraction, Sephadex LH-20 column chromatography, and high-speed countercurrent chromatography: A highly efficient strategy for the preparative separation of andrographolide from Andrographis paniculata in a single step.

PubMed

Zhang, Ying-Qi; Wang, Shan-Shan; Han, Chao; Xu, Jin-Fang; Luo, Jian-Guang; Kong, Ling-Yi

2017-12-01

A novel isolation strategy, online hyphenation of ultrasonic extraction, Sephadex LH-20 column chromatography combined with high-speed countercurrent chromatography, was developed for pure compounds extraction and purification. Andrographolide from Andrographis paniculata was achieved only in a single step purification protocol via the present strategy. The crude powder was ultrasonic extracted and extraction was pumped into Sephadex LH-20 column directly to cut the nontarget fractions followed by the second-dimensional high-speed countercurrent chromatography, hyphenated by a six-port valve equipped at the post-end of Sephadex LH-20 column, for the final purification. The results yielded andrographolide with the amount of 1.02 mg and a purity of 98.5% in a single step, indicating that the present method is effective to harvest target compound from medicinal plant. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Commissioning of the ECR ion source of the high intensity proton injector of the Facility for Antiproton and Ion Research (FAIR)

NASA Astrophysics Data System (ADS)

Tuske, O.; Chauvin, N.; Delferriere, O.; Fils, J.; Gauthier, Y.

2018-05-01

The CEA at Saclay is in charge of developing and building the ion source and the low energy line of the proton linac of the FAIR (Facility for Antiproton and Ion Research) accelerator complex located at GSI (Darmstadt) in Germany. The FAIR facility will deliver stable and rare isotope beams covering a huge range of intensities and beam energies for experiments in the fields of atomic physics, plasma physics, nuclear physics, hadron physics, nuclear matter physics, material physics, and biophysics. A significant part of the experimental program at FAIR is dedicated to antiproton physics that requires an ultimate number 7 × 1010 cooled pbar/h. The high-intensity proton beam that is necessary for antiproton production will be delivered by a dedicated 75 mA/70 MeV proton linac. A 2.45 GHz microwave ion source will deliver a 100 mA H+ beam pulsed at 4 Hz with an energy of 95 keV. A 2 solenoids low energy beam transport line allows the injection of the proton beam into the radio frequency quadrupole (RFQ) within an acceptance of 0.3π mm mrad (norm. rms). An electrostatic chopper system located between the second solenoid and the RFQ is used to cut the beam macro-pulse from the source to inject 36 μs long beam pulses into the RFQ. At present time, a Ladder-RFQ is under construction at the University of Frankfurt. This article reports the first beam measurements obtained since mid of 2016. Proton beams have been extracted from the ECR ion source and analyzed just after the extraction column on a dedicated diagnostic chamber. Emittance measurements as well as extracted current and species proportion analysis have been performed in different configurations of ion source parameters, such as magnetic field profile, radio frequency power, gas injection, and puller electrode voltage.

A poly(alkyl methacrylate-divinylbenzene-vinylbenzyl trimethylammonium chloride) monolithic column for solid-phase microextraction.

PubMed

Liu, Wan-Ling; Lirio, Stephen; Yang, Yicong; Wu, Lin-Tai; Hsiao, Shu-Ying; Huang, Hsi-Ya

2015-05-22

In this study, an organic polymer monolithic columns, which were prepared via in situ polymerization of alkyl methacrylate-ester (AMA), divinylbenzene (DVB) and vinylbenzyl trimethylammonium chloride (VBTA, charged monomer), were developed as adsorbent for solid-phase microextraction (SPME). Different parameters affecting the extraction efficiency for nine (9) non-steroidal anti-inflammatory drugs (NSAIDs) such as the ratio of the stearyl methacrylate (SMA) to DVB monomer, column length, sample pH, extraction flow rate and desorption solvent were investigated to obtain the optimal SPME condition. Also, the permeability for each poly(AMA-DVB-VBTA) monolithic column was investigated by adding porogenic solvent (poly(ethylene glycol), PEG). Using the optimized condition, a series of AMA-based poly(AMA-DVB-VBTA) monolith columns were developed to determine the effect the extraction efficiency of NSAIDs by varying the alkyl chain length of the methacrylate ester (methyl-, butyl-, octyl-, or lauryl-methacrylate; (MMA, BMA, OMA, LMA)). Results showed that decreasing the AMA chain length increases the extraction efficiency of some NSAIDs (i.e. sulindac (sul), naproxen (nap), ketoprofen (ket) and indomethacin (idm)). Among the poly(AMA-DVB-VBTA) monolithic columns, poly(BMA-DVB-VBTA) showed a highly repeatable extraction efficiency for NSAIDs with recoveries ranging from 85.0 to 100.2% with relative standard deviation (RSD) less than 6.8% (n=3). The poly(BMA-DVB-VBTA) can also be reused for at least 50 times without any significant effect in extraction efficiency for NSAIDs. Finally, using the established conditions, the poly(BMA-DVB-VBTA) was used to extract trace-level NSAIDs (100μgL(-1)) in river water with good recoveries ranging from 75.8 to 90.8% (RSD<14.9%). Copyright © 2015 Elsevier B.V. All rights reserved.

"Supermarket Column Chromatography of Leaf Pigments" Revisited: Simple and Ecofriendly Separation of Plant Carotenoids, Chlorophylls, and Flavonoids from Green and Red Leaves

ERIC Educational Resources Information Center

Dias, Alice M.; Ferreira, Maria La Salete

2015-01-01

A simple and ecofriendly procedure was developed in order to prepare extracts from red and green leaves. This procedure enables the separation of yellow, green, and red band pigments and optimizes the previously reported baking soda "supermarket column". The same extract also led to a novel and colorful potato starch column, which can…

40 CFR 1065.275 - N2O measurement devices.

Code of Federal Regulations, 2014 CFR

2014-07-01

... procedures for interpretation of infrared spectra. For example, EPA Test Method 320 is considered a valid... infrared analyzer. Examples of laser infrared analyzers are pulsed-mode high-resolution narrow band mid... for analysis. Examples of acceptable columns are a PLOT column consisting of bonded polystyrene...

40 CFR 1065.275 - N2O measurement devices.

Code of Federal Regulations, 2012 CFR

2012-07-01

... for interpretation of infrared spectra. For example, EPA Test Method 320 is considered a valid method... uncompensated signal's bias. Examples of laser infrared analyzers are pulsed-mode high-resolution narrow band.... Examples of acceptable columns are a PLOT column consisting of bonded polystyrene-divinylbenzene or a...

Trace analysis of impurities in bulk gases by gas chromatography-pulsed discharge helium ionization detection with "heart-cutting" technique.

PubMed

Weijun, Yao

2007-10-12

A method has been developed for the detection of low-nL/L-level impurities in bulk gases such as H(2), O(2), Ar, N(2), He, methane, ethylene and propylene, respectively. The solution presented here is based upon gas chromatography-pulsed discharge helium ionization detection (GC-PDHID) coupled with three two-position valves, one two-way solenoid valve and four packed columns. During the operation, the moisture and heavy compounds are first back-flushed via a pre-column. Then the trace impurities (except CO(2) which is diverted to a separate analytical column for separation and detection) together with the matrix enter onto a main column, followed by the heart-cut of the impurities onto a longer analytical column for complete separation. Finally the detection is performed by PDHID. This method has been applied to different bulk gases and the applicability of detecting impurities in H(2), Ar, and N(2) are herewith demonstrated. As an example, the resulting detection limit of 100 nL/L and a dynamic range of 100-1000 nL/L have been obtained using an Ar sample containing methane.

Calculation of extracted ion beam particle distribution including within-extractor collisions from H-alpha Doppler shift measurements.

PubMed

Kim, Tae-Seong; Kim, Jinchoon; In, Sang Ryul; Jeong, Seung Ho

2008-02-01

Prototype long pulse ion sources are being developed and tested toward the goal of a deuterium beam extraction of 120 keV/65 A. The latest prototype source consists of a magnetic bucket plasma generator and a four-grid copper accelerator system with multicircular apertures of 568 holes. To measure the angular divergence and the ion species of the ion beam, an optical multichannel analyzer (OMA) system for a Doppler-shifted H-alpha lights was set up at the end of a gas-cell neutralizer. But the OMA data are very difficult to analyze due to a large background level on the top of the three energy peaks (coming from H(+), H(2) (+), and H(3) (+)). These background spectra in the OMA signals seem to result from partially accelerated ion beams in the accelerator. Extracted ions could undergo a premature charge exchange as the accelerator column tends to have a high hydrogen partial pressure from the unused gas from the plasma generator, resulting in a continuous background of partially accelerated beam particles at the accelerator exit. This effect is calculated by accounting for all the possible atomic collision processes and numerically summing up three ion species across the accelerator column. The collection of all the atomic reaction cross sections and the numerical summing up will be presented. The result considerably depends on the background pressure and the ion beam species ratio (H(+), H(2) (+), and H(3) (+)). This effect constitutes more than 20% of the whole particle distribution. And the energy distribution of those suffering from collisions is broad and shows a broad maximum in the vicinity of the half and the third energy region.

Leaching of oxadyxil and tebuconazole in Colombian soil.

PubMed

Aldana, M; De Prado, R; Martínez, M J

2011-01-01

Lake Tota (Boyaca, Colombia) supplies water for human consumption, agriculture and industry for more than 500.000 people. Oxadixyl and Tebuconazole are fungicides used in onion crops in the lake catchment area. The mobility of pesticides in soil, bioavailability and transfer to other environmental compartments depend on sorption and desorption kinetics and mechanisms. An understanding of these processes is essential for transport modeling and the rational design of corrective measures against pollution. A displacement study was performed on a hand packed soil column in laboratory conditions. A pulse of 0,01 M CaCl2 solution, containing a tracer (Bromide) and the fungicides Oxadixyl y Tebuconazole, was injected. Column experiment was performed at 0.078 cmh(-1) flow rate under unsaturated conditions. Eluates were collected in flasks at constant intervals and the volumes of eluate were recorded. After rainfall simulation, the soil from the column was sliced into six successive sections (5 cm). Methanol extraction was used to determine the fungicide in each soil section. Samples were measured by HPLC. Only Oxadixyl was recovered in leachates. Unlike bromide breakthrough curve, Oxadixyl was asymmetrical, with early breakthrough and increased tailing. The percentage eluted was 96.7% after ten pore volumes. Tebuconazole showed the highest retention in the first five cm of soil layer. The results suggest that oxadyxil presents highs risk to leachate through the soil profile and that Tebuconazole is strongly absorbed in Colombian soil.

Determination of the Antibiotic Oxytetracycline in Commercial Milk by Solid-Phase Extraction: A High-Performance Liquid Chromatography (HPLC) Experiment for Quantitative Instrumental Analysis

ERIC Educational Resources Information Center

Mei-Ratliff, Yuan

2012-01-01

Trace levels of oxytetracylcine spiked into commercial milk samples are extracted, cleaned up, and preconcentrated using a C[subscript 18] solid-phase extraction column. The extract is then analyzed by a high-performance liquid chromatography (HPLC) instrument equipped with a UV detector and a C[subscript 18] column (150 mm x 4.6 mm x 3.5 [mu]m).…

Generalized Feature Extraction for Wrist Pulse Analysis: From 1-D Time Series to 2-D Matrix.

PubMed

Dimin Wang; Zhang, David; Guangming Lu

2017-07-01

Traditional Chinese pulse diagnosis, known as an empirical science, depends on the subjective experience. Inconsistent diagnostic results may be obtained among different practitioners. A scientific way of studying the pulse should be to analyze the objectified wrist pulse waveforms. In recent years, many pulse acquisition platforms have been developed with the advances in sensor and computer technology. And the pulse diagnosis using pattern recognition theories is also increasingly attracting attentions. Though many literatures on pulse feature extraction have been published, they just handle the pulse signals as simple 1-D time series and ignore the information within the class. This paper presents a generalized method of pulse feature extraction, extending the feature dimension from 1-D time series to 2-D matrix. The conventional wrist pulse features correspond to a particular case of the generalized models. The proposed method is validated through pattern classification on actual pulse records. Both quantitative and qualitative results relative to the 1-D pulse features are given through diabetes diagnosis. The experimental results show that the generalized 2-D matrix feature is effective in extracting both the periodic and nonperiodic information. And it is practical for wrist pulse analysis.

Histological examination of the oral mucosa after fractional diode laser irradiation with different power and pulse duration

NASA Astrophysics Data System (ADS)

Belikov, Andrey V.; Ermolaeva, Ludmila A.; Korzhevsky, Dmitriy E.; Sergeeva, Elena S.; Semyashkina, Yulia V.; Antropova, Maria M.; Fedotov, Denis Y.; Zaitseva, Maria A.; Kashina, Tatiana V.

2018-04-01

Optical and histological methods were used to examination of influence the power and pulse duration of 980-nm diode laser to the dimensions and morphology of tissue around fractional micro injuries created by the radiation of that laser in the oral mucosa of rats in vivo. The power of laser radiation (P) varied in the range of 1÷21 W, and its pulse duration (tp) - in the range 50÷500 ms. Histological examination showed that in the mucosa of the oral cavity after the laser fractional irradiation, there following effects are found: a tissue defect, a transudate in the lumen of ablative micro injury, stretching and compacting effect of the nuclei of the basal epithelium, the disappearance of granules of the keratohialin, destroying the structure of the connective tissue, erythrocyte stasis in the vessels, the disappearance of transverse striation in the muscle fibers in muscle layer. It has been found that ablative micro injury begins to form up at P = 5 W, tp = 100 ms and affects only the epithelial layer of the mucosa. At P = 7 W, tp = 120 ms, the ratio of width to depth of ablative micro injury is 1 : 1, and at P = 10 W, tp = 100 ms, an ablative micro column with ratio of 1 : 1.5 is formed in the epithelial and submucosal layers of the mucosa. The laser effect with P = 15 W, tp = 200 ms leads to lengthening of the ablation micro-column to 1 : 2, with the bottom of the ablative micro column reaching the muscular layer. With a further growth of laser power or pulse duration, the width of the micro injury increases, and the growth of the micro injury depth is slowed down so that the micro column buildup is ceased.

2-micron Double Pulsed IPDA Lidar for Atmospheric CO2 Measurement

NASA Astrophysics Data System (ADS)

Yu, Jirong; Petros, Mulugeta; Refaat, Tamer; Reithmaier, Karl; Remus, Ruben; Singh, Upendra; Johnson, Will; Boyer, Charlie; Fay, James; Johnston, Susan; Murchison, Luke; Scola, Tory

2015-04-01

We have developed a high energy pulsed 2-micron IPDA lidar instrument to measure the atmospheric CO2 column density. The IPDA lidar is operated on the long wavelength wing of R(30) CO2 line at 2050.967 nm (4875.749 cm-1) in the side-line operation mode. The R(30) line is an excellent absorption line for the measurements of CO2 in 2µm wavelength region with regard to the strength of the absorption lines, low susceptibility to atmospheric temperature variability, and freedom from problematic interference with other absorption lines. The Ho:Tm:YLF laser transmitter is designed to be operated in a unique double pulse format that can produce two-pulse pair in 10 Hz operation. Typically, the output energies of the laser transmitter are 100mJ and 45mJ for the first pulse and the second pulse, respectively. We injection seed the first pulse with on-line frequency and the second pulse with off-line frequency. The IPDA lidar instrument size, weight and power consumption were restricted to small research aircraft payload requirements. The airborne IPDA lidar instrument measures the total integrated column content of CO2 from the instrument to the ground but with weighting that can be tuned by controlling the transmitted wavelengths. Therefore, the transmitter could be tuned to weight the column measurement to the surface for optimum CO2 interaction studies or up to the free troposphere for optimum transport studies. The 2-μm CO2 IPDA lidar airborne demonstration was conducted during March 20, 2014 through April 10, 2014. IPDA lidar airborne flights included various operating and environmental conditions. Environmental conditions included different flight altitude up to 8.3 km, different ground target conditions such as vegetation, soil, ocean, snow and sand and different cloud conditions. Besides, some flights targeted power plant incinerators for investigating the IPDA sensitivity to CO2 plums. The lidar instrument is robust during all of the flights. This paper describes the development of the new 2-micron pulsed IPDA lidar instrument, and presents the initial data for the airborne measurements of atmospheric CO2 concentration.

Automated clean-up, separation and detection of polycyclic aromatic hydrocarbons in particulate matter extracts from urban dust and diesel standard reference materials using a 2D-LC/2D-GC system.

PubMed

Ahmed, Trifa M; Lim, Hwanmi; Bergvall, Christoffer; Westerholm, Roger

2013-10-01

A multidimensional, on-line coupled liquid chromatographic/gas chromatographic system was developed for the quantification of polycyclic aromatic hydrocarbons (PAHs). A two-dimensional liquid chromatographic system (2D-liquid chromatography (LC)), with three columns having different selectivities, was connected on-line to a two-dimensional gas chromatographic system (2D-gas chromatography (GC)). Samples were cleaned up by combining normal elution and column back-flush of the LC columns to selectively remove matrix constituents and isolate well-defined, PAH enriched fractions. Using this system, the sequential removal of polar, mono/diaromatic, olefinic and alkane compounds from crude extracts was achieved. The LC/GC coupling was performed using a fused silica transfer line into a programmable temperature vaporizer (PTV) GC injector. Using the PTV in the solvent vent mode, excess solvent was removed and the enriched PAH sample extract was injected into the GC. The 2D-GC setup consisted of two capillary columns with different stationary phase selectivities. Heart-cutting of selected PAH compounds in the first GC column (first dimension) and transfer of these to the second GC column (second dimension) increased the baseline resolutions of closely eluting PAHs. The on-line system was validated using the standard reference materials SRM 1649a (urban dust) and SRM 1975 (diesel particulate extract). The PAH concentrations measured were comparable to the certified values and the fully automated LC/GC system performed the clean-up, separation and detection of PAHs in 16 extracts in less than 24 h. The multidimensional, on-line 2D-LC/2D-GC system eliminated manual handling of the sample extracts and minimised the risk of sample loss and contamination, while increasing accuracy and precision.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of semivolatile organic compounds in bottom sediment by solvent extraction, gel permeation chromatographic fractionation, and capillary-column gas chromatography/mass spectrometry

USGS Publications Warehouse

Furlong, E.T.; Vaught, D.G.; Merten, L.M.; Foreman, W.T.; Gates, Paul M.

1996-01-01

A method for the determination of 79 semivolatile organic compounds (SOCs) and 4 surrogate compounds in soils and bottom sediment is described. The SOCs are extracted from bottom sediment by solvent extraction, followed by partial isolation using high-performance gel permeation chromatography (GPC). The SOCs then are qualitatively identified and quantitative concentrations determined by capillary-column gas chromatography/mass spectrometry (GC/MS). This method also is designed for an optional simultaneous isolation of polychlorinated biphenyls (PCBs) and organochlorine (OC) insecticides, including toxaphene. When OCs and PCBs are determined, an additional alumina- over-silica column chromatography step follows GPC cleanup, and quantitation is by dual capillary- column gas chromatography with electron-capture detection (GC/ECD). Bottom-sediment samples are centrifuged to remove excess water and extracted overnight with dichloromethane. The extract is concentrated, centrifuged, and then filtered through a 0.2-micrometer polytetrafluoro-ethylene syringe filter. Two aliquots of the sample extract then are quantitatively injected onto two polystyrene- divinylbenzene GPC columns connected in series. The SOCs are eluted with dichloromethane, a fraction containing the SOCs is collected, and some coextracted interferences, including elemental sulfur, are separated and discarded. The SOC-containing GPC fraction then is analyzed by GC/MS. When desired, a second aliquot from GPC is further processed for OCs and PCBs by combined alumina-over-silica column chromatography. The two fractions produced in this cleanup then are analyzed by GC/ECD. This report fully describes and is limited to the determination of SOCs by GC/MS.

Automated solid-phase extraction and liquid chromatography for assay of cyclosporine in whole blood.

PubMed

Kabra, P M; Wall, J H; Dimson, P

1987-12-01

In this rapid, precise, accurate, cost-effective, automated liquid-chromatographic procedure for determining cyclosporine in whole blood, the cyclosporine is extracted from 0.5 mL of whole blood together with 300 micrograms of cyclosporin D per liter, added as internal standard, by using an Advanced Automated Sample Processing unit. The on-line solid-phase extraction is performed on an octasilane sorbent cartridge, which is interfaced with a RP-8 guard column and an octyl analytical column, packed with 5-microns packing material. Both columns are eluted with a mobile phase containing acetonitrile/methanol/water (53/20/27 by vol) at a flow rate of 1.5 mL/min and column temperature of 70 degrees C. Absolute recovery of cyclosporine exceeded 85% and the standard curve was linear to 5000 micrograms/L. Within-run and day-to-day CVs were less than 8%. Correlation between automated and manual Bond-Elut extraction methods was excellent (r = 0.987). None of 18 drugs and four steroids tested interfered.

Preparation and evaluation of a mixed-bed immunoaffinity column for selective purification of sixteen sulfonamides in pork muscle.

PubMed

Li, Yingguo; Chen, Yiqiang; Li, Zhengguo; Zhang, Lei; Li, Xianliang; Xi, Cunxian; Wang, Guomin; Wang, Xiong; Guo, Qi; Li, Na

2012-03-01

This paper describes the preparation of a novel mixed-bed immunoaffinity chromatography (IAC) column by coupling four monoclonal antibodies against different sulfonamides (SAs) to Sepharose 4B. The IAC column can be used to simultaneously extract and purify 16 SAs in pork muscle. The dynamic column capacities for all SAs in mixed standard solution were between 312 and 479 ng/mL gel. After simple extraction and IAC cleanup, the sample solution can be directly injected for liquid chromatography-ultraviolet analysis. The recoveries of SAs from spiked samples at levels of 25, 50 and 100 µg/kg ranged from 83.3 to 103.1% with variation coefficient less than 8.6%. The comparison of IAC with liquid-liquid extraction and solid phase extraction indicated that IAC has better purification effect and needs less organic solution than conventional methods, thus it would be an ideal method for selective purification of SAs in pork muscle.

A novel approach to the simultaneous extraction and non-targeted analysis of the small molecules metabolome and lipidome using 96-well solid phase extraction plates with column-switching technology.

PubMed

Li, Yubo; Zhang, Zhenzhu; Liu, Xinyu; Li, Aizhu; Hou, Zhiguo; Wang, Yuming; Zhang, Yanjun

2015-08-28

This study combines solid phase extraction (SPE) using 96-well plates with column-switching technology to construct a rapid and high-throughput method for the simultaneous extraction and non-targeted analysis of small molecules metabolome and lipidome based on ultra-performance liquid chromatography quadrupole time-of-flight mass spectrometry. This study first investigated the columns and analytical conditions for small molecules metabolome and lipidome, separated by an HSS T3 and BEH C18 columns, respectively. Next, the loading capacity and actuation duration of SPE were further optimized. Subsequently, SPE and column switching were used together to rapidly and comprehensively analyze the biological samples. The experimental results showed that the new analytical procedure had good precision and maintained sample stability (RSD<15%). The method was then satisfactorily applied to more widely analyze the small molecules metabolome and lipidome to test the throughput. The resulting method represents a new analytical approach for biological samples, and a highly useful tool for researches in metabolomics and lipidomics. Copyright © 2015 Elsevier B.V. All rights reserved.

A Column Experiment To Determine Black Shale Degradation And Colonization By Means of δ13C and 14C Analysis Of Phospholipid Fatty Acids And DNA Extraction

NASA Astrophysics Data System (ADS)

Seifert, A.; Gleixner, G.

2008-12-01

We investigated the degradation of black shale organic matter by microbial communities. We inoculated two columns respectively, with the fungi Schizophyllum commune, the gram-positive bacterium Pseudomonas putida and the gram-negative bacteria Streptomyces griseus and Streptomyces chartreusis. These microorganisms are known to degrade a wide variety of organic macromolecules. Additionally, we had two sets of control columns. To one set the same nutrient solution was added as to the inoculated columns and to the other set only sterile deionised water was supplied. All columns contained 1.5 kg of freshly crushed not autoclaved black shale material with a particle size of 0.63-2 mm. The columns were incubated at 28° C and 60% humidity in the dark. The aim was to investigate, which microorganisms live on black shales and if these microorganisms are able to degrade ancient organic matter. We used compound specific stable isotope measurement techniques and compound specific 14C-dating methods. After 183 days PLFAs were extracted from the columns to investigate the microbial community, furthermore we extracted on one hand total-DNA of column material and on the other hand DNA from pure cultures isolates which grew on Kinks-agar B, Starch-casein-nitrate-agar (SCN) and on complete-yeast-medium-agar (CYM). According to the PLFA analysis bacteria dominated in the columns, whereas in pure cultures more fungi were isolated. A principal component analysis revealed differences between the columns in accordance with the inoculation, but it seems that the inoculated microorganisms were replaced by the natural population. For AMS measurements palmitic acid (C 16:0) was re-isolated from total-PLFA-extract with a preparative fraction collector (PFC). Preliminary results of the study revealed that microorganisms are able to degrade black shale material and that PLFA analysis are useful methods to be combined with analysis of stable isotope and 14C measurements to study microbial degradation processes.

Airborne Measurements of CO2 Column Absorption and Range Using a Pulsed Direct-Detection Integrated Path Differential Absorption Lidar

NASA Technical Reports Server (NTRS)

Abshire, James B.; Riris, Haris; Weaver, Clark J.; Mao, Jianping; Allan, Graham R.; Hasselbrack, William E.; Browell, Edward V.

2013-01-01

We report on airborne CO2 column absorption measurements made in 2009 with a pulsed direct-detection lidar operating at 1572.33 nm and utilizing the integrated path differential absorption technique. We demonstrated these at different altitudes from an aircraft in July and August in flights over four locations in the central and eastern United States. The results show clear CO2 line shape and absorption signals, which follow the expected changes with aircraft altitude from 3 to 13 km. The lidar measurement statistics were also calculated for each flight as a function of altitude. The optical depth varied nearly linearly with altitude, consistent with calculations based on atmospheric models. The scatter in the optical depth measurements varied with aircraft altitude as expected, and the median measurement precisions for the column varied from 0.9 to 1.2 ppm. The altitude range with the lowest scatter was 810 km, and the majority of measurements for the column within it had precisions between 0.2 and 0.9 ppm.

Quantitation of promethazine and metabolites in urine samples using on-line solid-phase extraction and column-switching

NASA Technical Reports Server (NTRS)

Song, Q.; Putcha, L.; Harm, D. L. (Principal Investigator)

2001-01-01

A chromatographic method for the quantitation of promethazine (PMZ) and its three metabolites in urine employing on-line solid-phase extraction and column-switching has been developed. The column-switching system described here uses an extraction column for the purification of PMZ and its metabolites from a urine matrix. The extraneous matrix interference was removed by flushing the extraction column with a gradient elution. The analytes of interest were then eluted onto an analytical column for further chromatographic separation using a mobile phase of greater solvent strength. This method is specific and sensitive with a range of 3.75-1400 ng/ml for PMZ and 2.5-1400 ng/ml for the metabolites promethazine sulfoxide, monodesmethyl promethazine sulfoxide and monodesmethyl promethazine. The lower limits of quantitation (LLOQ) were 3.75 ng/ml with less than 6.2% C.V. for PMZ and 2.50 ng/ml with less than 11.5% C.V. for metabolites based on a signal-to-noise ratio of 10:1 or greater. The accuracy and precision were within +/- 11.8% in bias and not greater than 5.5% C.V. in intra- and inter-assay precision for PMZ and metabolites. Method robustness was investigated using a Plackett-Burman experimental design. The applicability of the analytical method for pharmacokinetic studies in humans is illustrated.

Phenylboronic acid modified solid-phase extraction column: Preparation, characterization, and application to the analysis of amino acids in sepia capsule by removing the maltose.

PubMed

Guo, Mengzhe; Yin, Dengyang; Han, Jie; Zhang, Liyan; Li, Xiao; He, Dandan; Du, Yan; Tang, Daoquan

2016-09-01

Maltose, a common auxiliary material of pharmaceutical preparation, may disturb the analysis of total amino acids in sepia capsule by aldolization. Therefore, it is necessary to remove the maltose through a convenient method. In this work, a phenylboronic acid modified solid-phase extraction column has been synthesized and used to remove the maltose. The materials were synthesized by one step "thiol-ene" reaction and the parameters of the column such as absorption capacity, recovery, and absorption specificity have been investigated. The results showed the column (0.5 cm of length × 0.5 cm of inner diameter) can absorb 4.6 mg maltose with a linear absorption and absorption specificity. Then this technique was applied in the quantification of amino acids in sepia capsule. After the optimization of the method, four kinds of amino acids, which were the most abundant, were quantified by high-performance liquid chromatography with diode array detection. The amounts of the four kinds of amino acids are 1.5∼2 times more than that without the treatment of solid-phase extraction column, which almost overcomes the influence of the maltose. All the results indicate that the phenylboronic acid modified solid-phase extraction column can successfully help to accurately quantify the total amino acids in sepia capsule. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Measurement of Atmospheric CO2 Column Concentrations to Cloud Tops With a Pulsed Multi-Wavelength Airborne Lidar

NASA Technical Reports Server (NTRS)

Mao, Jianping; Ramanathan, Anand; Abshire, James B.; Kawa, Stephan R.; Riris, Haris; Allan, Graham R.; Rodriguez, Michael R.; Hasselbrack, William E.; Sun, Xiaoli; Numata, Kenji;

Measurement of atmospheric CO2 column concentrations to cloud tops with a pulsed multi-wavelength airborne lidar

NASA Astrophysics Data System (ADS)

Mao, Jianping; Ramanathan, Anand; Abshire, James B.; Kawa, Stephan R.; Riris, Haris; Allan, Graham R.; Rodriguez, Michael; Hasselbrack, William E.; Sun, Xiaoli; Numata, Kenji; Chen, Jeff; Choi, Yonghoon; Yang, Mei Ying Melissa

2018-01-01

We have measured the column-averaged atmospheric CO2 mixing ratio to a variety of cloud tops by using an airborne pulsed multi-wavelength integrated-path differential absorption (IPDA) lidar. Airborne measurements were made at altitudes up to 13 km during the 2011, 2013 and 2014 NASA Active Sensing of CO2 Emissions over Nights, Days, and Seasons (ASCENDS) science campaigns flown in the United States West and Midwest and were compared to those from an in situ sensor. Analysis of the lidar backscatter profiles shows the average cloud top reflectance was ˜ 5 % for the CO2 measurement at 1572.335 nm except to cirrus clouds, which had lower reflectance. The energies for 1 µs wide laser pulses reflected from cloud tops were sufficient to allow clear identification of CO2 absorption line shape and then to allow retrievals of atmospheric column CO2 from the aircraft to cloud tops more than 90 % of the time. Retrievals from the CO2 measurements to cloud tops had minimal bias but larger standard deviations when compared to those made to the ground, depending on cloud top roughness and reflectance. The measurements show this new capability helps resolve CO2 horizontal and vertical gradients in the atmosphere. When used with nearby full-column measurements to ground, the CO2 measurements to cloud tops can be used to estimate the partial-column CO2 concentration below clouds, which should lead to better estimates of surface carbon sources and sinks. This additional capability of the range-resolved CO2 IPDA lidar technique provides a new benefit for studying the carbon cycle in future airborne and space-based CO2 missions.

Optimized extraction of polysaccharides from corn silk by pulsed electric field and response surface quadratic design.

PubMed

Zhao, Wenzhu; Yu, Zhipeng; Liu, Jingbo; Yu, Yiding; Yin, Yongguang; Lin, Songyi; Chen, Feng

2011-09-01

Corn silk is a traditional Chinese herbal medicine, which has been widely used for treatment of some diseases. In this study the effects of pulsed electric field on the extraction of polysaccharides from corn silk were investigated. Polysaccharides in corn silk were extracted by pulsed electric field and optimized by response surface methodology (RSM), based on a Box-Behnken design (BBD). Three independent variables, including electric field intensity (kV cm(-1) ), ratio of liquid to raw material and pulse duration (µs), were investigated. The experimental data were fitted to a second-order polynomial equation and also profiled into the corresponding 3-D contour plots. Optimal extraction conditions were as follows: electric field intensity 30 kV cm(-1) , ratio of liquid to raw material 50, and pulse duration 6 µs. Under these condition, the experimental yield of extracted polysaccharides was 7.31% ± 0.15%, matching well with the predicted value. The results showed that a pulsed electric field could be applied to extract value-added products from foods and/or agricultural matrix. Copyright © 2011 Society of Chemical Industry.

ANALYSIS OF FERRIC AND FERROUS IONS IN SOIL EXTRACTS BY ION CHROMATOGRAPHY

EPA Science Inventory

A method using ion chromatography (IC) for the analysis of ferrous (Fe 2+) and ferric (Fe 3+) ions in soil extracts has been developed. This method uses an ion exchange column with detection at 520 nm after post-column derivatization. Selectivity is achieved by using an anionic...

[Determination of patulin in fruits and jam by solid phase extraction-ultra performance liquid chromatography].

PubMed

Lü, Weichao; Shen, Shuchang; Wang, Chao

2017-11-08

With magnesium silicate, silica gel, diatomite and calcium sulfate as raw materials, a new solid phase extraction column was prepared through a series of processes of grinding to ethanol homogenate, drying and packing into polypropylene tube. The sample was hydrolyzed by pectinase, extracted by acetonitrile and purified by solid phase extraction. The target compounds were separated on a C18 column (100 mm×2.1 mm, 1.8 μm), using 0.8% (v/v) tetrahydrofuran solution as mobile phase with a flow rate of 0.5 mL/min. The detection wavelength was 276 nm. The effect of pectinase on extraction yield and purification effect of solid-phase extraction column were investigated. The optimum chromatographic conditions were selected. There was a good linear relationship between the peak heights and the mass concentrations of patulin in the range of 0.1 to 10 mg/L with the correlation coefficient ( R 2 ) of 1. The limit of detection for this method was 10.22 μg/kg. The spiked recoveries of samples were 86.58%-94.84% with the relative standard deviations (RSDs) of 1.45%-2.28%. The results indicated that the self-made solid phase extraction column had a good purification efficiency, and the UPLC had a high separation efficiency. The method is simple, accurate and of great significance for the quality and safety control of fruit products.

Drawing Blueprints for "Pulsing Content" Libraries

ERIC Educational Resources Information Center

Chudnov, Daniel

2007-01-01

This column presents a continuation of an article published in last month's issue of "Libraries in Computers," in which the author began to consider what it might mean to build dynamic, instantaneous libraries based solely on the materials held on the computers of people in the same space. The goal of this column is to think about what libraries…

Synoptic events force biological productivity in Patagonian fjord ecosystems

NASA Astrophysics Data System (ADS)

Daneri, Giovanni

2016-04-01

The annual cycle of primary productivity of the Patagonian fjords has, to date, been described as a two phase system consisting of a short non productive winter phase (during June and July) and a productive phase extending from late winter (August) to autumn (May). Low levels of primary production, phytoplankton biomass and high concentrations of surface nutrients have been described as characterizing winter conditions while pulsed productivity events typifies the productivity pattern during the extended productive season. Pulsed productivity events characterize coastal waters where inorganic nutrients in surface layers are replenished following periods of intensive utilization by autotrophs. Freshwater input in Patagonian fjords in southern Chile (41-55°S) results in one of the largest estuarine regions worldwide. Here strong haline water column stratification prevents nutrient mixing to the surface layers thus potentially shutting off algal production. Our working hypothesis considered that in order to reconcile the observed pulsed productivity pattern, periodic breaking (associated to surface nutrient replenishment) and re-establishment of estuarine conditions (associated to water column stratification) would be required. Up to now however our understanding of the physical processes that control water column conditions in the Patagonian fjord area has been extremely limited. Here we present evidence linking the passage of synoptic low pressure fronts to pulsed productivity events in the Patagonian fjord area. These front controls and influence local processes of interaction between the fjord and the atmosphere generating a rapid water column response. In the specific case of the Puyuhuapi fjord we have been able to show that such synoptic fronts induce surface flow reversal and water column mixing. Phytoplankton blooming occurs after the passage of the synoptic front once calmer conditions prevail and estuarine conditions are re established. The occurrence of an extremely productive bloom of the dinoflagellate Heterocapsa sp. in July 2014, after the passage of a synoptic low pressure front provided, for the first time, strong evidence that phytoplankton blooming in the Patagonian fjord ecosystems is controlled by synoptic processes and that they are not limited by light as previously reported. This research was funded by COPAS Sur-Austral (PFB-31) and FONDECYT 1131063

Determination of biogenic amines in chocolate by ion chromatographic separation and pulsed integrated amperometric detection with implemented wave-form at Au disposable electrode.

PubMed

Pastore, Paolo; Favaro, Gabriella; Badocco, Denis; Tapparo, Andrea; Cavalli, Silvano; Saccani, Giovanna

2005-12-09

A rapid and selective cation exchange chromatographic method coupled to integrated pulsed amperometric detection (PAD) has been developed to quantify biogenic amines in chocolate. The method is based on gradient elution of aqueous methanesulfonic acid with post column addition of strong base to obtain suitable conditions for amperometric detection. A potential waveform able to keep long time performance of the Au disposable electrode was set up. Total analysis time is less than 20min. Concentration levels of dopamine, serotonin, tyramine, histamine and 2-phenylethylamine were measured, after extraction with perchloric acid from 2g samples previously defatted twice with petroleum ether. The method was used to determine the analytes in chocolate real matrices and their quantification was made with standard addition method. Only dopamine, histamine and serotonin were found in the analysed real samples. Repeatabilities of their signals, computed on their amounts in the real samples, were 5% for all of them. Repeatabilities of tyramine and phenethylamine were relative to standard additions to real samples (close to 1mg/l in the extract) and were 7 and 3%, respectively. Detection limits were computed with the 3s of the baseline noise combined with the calibration plot regression parameters. They were satisfactorily low for all amines: 3mg/kg for dopamine, 2mg/kg for tyramine, 1mg/kg for histamine, 2mg/kg for serotonin, 3mg/kg for 2-phenylethylamine.

Liquid-chromatographic analysis for cyclosporine with use of a microbore column and small sample volume.

PubMed

Annesley, T; Matz, K; Balogh, L; Clayton, L; Giacherio, D

1986-07-01

This liquid-chromatographic assay requires 0.2 to 0.5 mL of whole blood, avoids the use of diethyl ether, and consumes only 10 to 20% of the solvents used in prior methods. Sample preparation involves an acidic extraction with methyl-t-butyl ether, performed in a 13 X 100 mm disposable glass tube, then a short second extraction of the organic phase with sodium hydroxide. After evaporation of the methyl-t-butyl ether, chromatography is performed on an "Astec" 2.0-mm (i.d.) octyl column. We compared results by this procedure with those by use of earlier larger-scale extractions and their respective 4.6-mm (i.d.) columns; analytical recoveries of cyclosporins A and D were comparable with previous findings and results for patients' specimens were equivalent, but the microbore columns provided greatly increased resolution and sensitivity.

Multi-Pulse Extraction from Los Alamos Proton Storage Ring for Radiographic Applications

NASA Astrophysics Data System (ADS)

Thiessen, Henry A.; Neri, Filippo; Rust, Kenneth R.; Redd, Dale B.

1997-05-01

For radiography of moving objects, two or more pulses with adjustable time spacing are required. The existing Proton Stotage Ring (PSR) extraction system is configured to extract the entire beam in a single turn. Two kickers and two kicker modulators fired at the same time perform the normal extraction function. By reconfiguring the two kickers and two modulators, it is possible to obtain two half-sized extraction kicks with adjustable time spacing. In this way, we have extracted two pulses with adjustable relative timing. The setup will be described and experimental results will be presented.

Determination of Low Concentrations of Acetochlor in Water by Automated Solid-Phase Extraction and Gas Chromatography with Mass-Selective Detection

USGS Publications Warehouse

Lindley, C.E.; Stewart, J.T.; Sandstrom, M.W.

1996-01-01

A sensitive and reliable gas chromatographic/mass spectrometric (GC/MS) method for determining acetochlor in environmental water samples was developed. The method involves automated extraction of the herbicide from a filtered 1 L water sample through a C18 solid-phase extraction column, elution from the column with hexane-isopropyl alcohol (3 + 1), and concentration of the extract with nitrogen gas. The herbicide is quantitated by capillary/column GC/MS with selected-ion monitoring of 3 characteristic ions. The single-operator method detection limit for reagent water samples is 0.0015 ??g/L. Mean recoveries ranged from about 92 to 115% for 3 water matrixes fortified at 0.05 and 0.5 ??g/L. Average single-operator precision, over the course of 1 week, was better than 5%.

Split Flow Online Solid-Phase Extraction Coupled with Inductively Coupled Plasma Mass Spectrometry System for One-Shot Data Acquisition of Quantification and Recovery Efficiency.

PubMed

Furukawa, Makoto; Takagai, Yoshitaka

2016-10-04

Online solid-phase extraction (SPE) coupled with inductively coupled plasma mass spectrometry (ICPMS) is a useful tool in automatic sequential analysis. However, it cannot simultaneously quantify the analytical targets and their recovery percentages (R%) in one-shot samples. We propose a system that simultaneously acquires both data in a single sample injection. The main flowline of the online solid-phase extraction is divided into main and split flows. The split flow line (i.e., bypass line), which circumvents the SPE column, was placed on the main flow line. Under program-controlled switching of the automatic valve, the ICPMS sequentially measures the targets in a sample before and after column preconcentration and determines the target concentrations and the R% on the SPE column. This paper describes the system development and two demonstrations to exhibit the analytical significance, i.e., the ultratrace amounts of radioactive strontium ( 90 Sr) using commercial Sr-trap resin and multielement adsorbability on the SPE column. This system is applicable to other flow analyses and detectors in online solid phase extraction.

Pretreatment method for immunoassay of polychlorinated biphenyls in transformer oil using multilayer capillary column and microfluidic liquid-liquid partitioning.

PubMed

Aota, Arata; Date, Yasumoto; Terakado, Shingo; Ohmura, Naoya

2013-01-01

Polychlorinated biphenyls (PCBs) are persistent organic pollutants that are present in the insulating oil inside a large number of transformers. To aid in eliminating PCB-contaminated transformers, PCBs in oil need to be measured using a rapid and cost-effective analytical method. We previously reported a pretreatment method for the immunoassay of PCBs in oil using a large-scale multilayer column and a microchip with multiple microrecesses, which permitted concentrated solvent extraction. In this paper, we report on a more rapid and facile pretreatment method, without an evaporation process, by improving the column and the microchip. In a miniaturized column, the decomposition and separation of oil were completed in 2 min. PCBs can be eluted from the capillary column at concentrations seven-times higher than those from the previous column. The total volume of the microrecesses was increased by improving the microrecess structure, the enabling extraction of four-times the amount of PCBs achieved with the previous system. By interfacing the capillary column with the improved microchip, PCBs in the eluate from the column were extracted into dimethyl sulfoxide in microrecesses with high enrichment and without the need for evaporation. Pretreatment was completed within 20 min. The pretreated oil was analyzed using a flow-based kinetic exclusion immunoassay. The limit of detection of PCBs in oil was 0.15 mg kg(-1), which satisfies the criterion set in Japan of 0.5 mg kg(-1).

Blind column selection protocol for two-dimensional high performance liquid chromatography.

PubMed

Burns, Niki K; Andrighetto, Luke M; Conlan, Xavier A; Purcell, Stuart D; Barnett, Neil W; Denning, Jacquie; Francis, Paul S; Stevenson, Paul G

2016-07-01

The selection of two orthogonal columns for two-dimensional high performance liquid chromatography (LC×LC) separation of natural product extracts can be a labour intensive and time consuming process and in many cases is an entirely trial-and-error approach. This paper introduces a blind optimisation method for column selection of a black box of constituent components. A data processing pipeline, created in the open source application OpenMS®, was developed to map the components within the mixture of equal mass across a library of HPLC columns; LC×LC separation space utilisation was compared by measuring the fractional surface coverage, fcoverage. It was found that for a test mixture from an opium poppy (Papaver somniferum) extract, the combination of diphenyl and C18 stationary phases provided a predicted fcoverage of 0.48 and was matched with an actual usage of 0.43. OpenMS®, in conjunction with algorithms designed in house, have allowed for a significantly quicker selection of two orthogonal columns, which have been optimised for a LC×LC separation of crude extractions of plant material. Copyright © 2016 Elsevier B.V. All rights reserved.

Polymeric monolith column composited with multiwalled carbon nanotubes-β-cyclodextrin for the selective extraction of psoralen and isopsoralen.

PubMed

Ling, Xu; Zou, Li; Chen, Zilin

2017-09-01

A polymeric column that contains multiwalled carbon nanotubes-β-cyclodextrin composite was developed. The composite was wrapped into the poly(butyl methacrylate-ethylene dimethacrylate) monolith column (0.76 mm id and 10 cm in length). The column was then applied for the online solid-phase microextraction of psoralen and isopsoralen from Fructus Psoraleae. Following microextraction, the coumarins were quantified by high-performance liquid chromatography with C 18 separation column and UV detection. The effects of sample flow rate, sample volume, and pH value were optimized. The method showed low limits of detection (20 pg/mL, S/N = 3) for both psoralen and isopsoralen. Finally the method was successfully applied to the determination of psoralen and isopsoralen in spiked herb extracts and rat plasma where it gave recoveries that ranged between 93.2 and 102.1%. The empty hydrophobic cavities of β-cyclodextrin and the hydrophobicity of multiwalled carbon nanotubes provided specific extraction capability for psoralen and isopsoralen. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Removal of Cryptosporidium parvum in bank filtration systems

NASA Astrophysics Data System (ADS)

Harter, T.; Atwill, E. R.; Hou, L. L.

2003-04-01

The protozoan pathogen Cryptosporidium parvum is a leading cause of waterborne disease. Many surface water systems therefore depend on filtration systems, including bank filtration systems, for the removal of the pathogenic oocysts. To better understand the effectiveness, e.g., of bank filtration systems, we have implemented a series of columns studies under various environmental conditions (column length: 10 cm - 60 cm, flow rates: 0.7 m/d - 30 m/d, ionic strength: 0.01 - 100 mM, filter grain size: 0.2 - 2 mm, various solution chemistry). We show that classic colloid filtration theory is a reasonable tool for predicting the initial breakthrough of C. parvum in pulsed injections of the oocyst through sand columns, although the model does not account for the significant tailing that occurs in C. parvum transport. Application of colloid filtration theory to bank filtration system is further limited by the intrinsic heterogeneity of the geologic systems used for bank filtration. We couple filtration theory with a stochastic subsurface transport approach and with percolation theory to account for the effects of intrinsic heterogeneity. We find that a 1-log removal can be achieved even under relatively adverse conditions (low collision efficiency, high velocity) if 85% - 90% of the sedimentary hydrofacies located within the bank filtration system or of the coarsest known hydrofacies connecting the riverbed with the extraction system has a grain-size distribution with a 10% passing diameter equal to 1 mm. One millimeter is a standard sieve size in sediment analysis.

Methods of Analysis by the U.S. Geological Survey National Water Quality Laboratory - Determination of Moderate-Use Pesticides and Selected Degradates in Water by C-18 Solid-Phase Extraction and Gas Chromatography/Mass Spectrometry

USGS Publications Warehouse

Sandstrom, Mark W.; Stroppel, Max E.; Foreman, William T.; Schroeder, Michael P.

2001-01-01

A method for the isolation and analysis of 21 parent pesticides and 20 pesticide degradates in natural-water samples is described. Water samples are filtered to remove suspended particulate matter and then are pumped through disposable solid-phase-extraction columns that contain octadecyl-bonded porous silica to extract the analytes. The columns are dried by using nitrogen gas, and adsorbed analytes are eluted with ethyl acetate. Extracted analytes are determined by capillary-column gas chromatography/mass spectrometry with selected-ion monitoring of three characteristic ions. The upper concentration limit is 2 micrograms per liter (?g/L) for most analytes. Single-operator method detection limits in reagent-water samples range from 0.00 1 to 0.057 ?g/L. Validation data also are presented for 14 parent pesticides and 20 degradates that were determined to have greater bias or variability, or shorter holding times than the other compounds. The estimated maximum holding time for analytes in pesticide-grade water before extraction was 4 days. The estimated maximum holding time for analytes after extraction on the dry solid-phase-extraction columns was 7 days. An optional on-site extraction procedure allows for samples to be collected and processed at remote sites where it is difficult to ship samples to the laboratory within the recommended pre-extraction holding time. The method complements existing U.S. Geological Survey Method O-1126-95 (NWQL Schedules 2001 and 2010) by using identical sample preparation and comparable instrument analytical conditions so that sample extracts can be analyzed by either method to expand the range of analytes determined from one water sample.

Development of a rapid screening technique for organochlorine pesticides using solvent microextraction (SME) and fast gas chromatography (GC).

PubMed

de Jager, L S; Andrews, A R

2000-11-01

A novel, fast screening method for organochlorine pesticides (OCPs) in water samples has been developed. Total analysis time was less than 9 min, allowing 11 samples to be screened per hour. The relatively new technique of solvent microextraction (SME) was used to extract and preconcentrate the pesticides into a single drop of hexane. The use of a conventional carbon dioxide cryotrap was investigated for introduction of the extract onto a micro-bore (0.1 mm) capillary column for fast GC analysis. A pulsed-discharge electron capture detector was used which yielded selective and sensitive measurement of the pesticide peaks. Fast GC conditions were optimised and tested with the previously developed SME procedure. Calibration curves yielded good linearity and concentrations down to 0.25 ng mL-1 were detectable with RSD values ranging from 12.0 to 28% and LOD for most OCPs at 0.25 ng mL-1. Spiked river water samples were tested and using the developed screen we were able to differentiate between spiked samples and samples containing no OCPs.

EVALUATION OF AUSTRALIAN RUM JUNGLE URANIUM CONCENTRATE FOR USE AS NLO REFINERY FEED

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

Collopy, T.J.; Huntington, C.W.; Blum, J.F.

1956-01-20

A laboratory evaluation of Australian Rum Jungle uranium concentrate showed that the uracium can be satisfactorily extracted by 33.5% TBP-kerosene from an aqueous acid slurry of the material, and that impurities in the aqueous uranyl nitrate product obtained by re-extraetion from the organic phase approach NL0 tolerance specifications. The uranium values in the organic product were not completely re-extracted at room temperatare (l0th stage organic, 1.6 g/l U); however, it was assumed that reextraction will be complete under pulse column conditions (150 deg F). The results of the Pilot Plant evaluation of Rum Jungle uranium concentrate (Lot No. 1) indicatedmore » that this material can be processed employing NLO refinery conditions. The aqueous uranyl nitrate product from the test met all impurity specifications except those for manganese and nickel. The high chloride content of this lot of concentrate will mske blending necessary in order to meet NLO feed material specifications. The blending will alan lessen the tendencies toward metallic contamination of the OK liquor observed in these tests. (auth)« less

Effects of a malfunctional column on conventional and FeedCol-simulated moving bed chromatography performance.

PubMed

Song, Ji-Yeon; Oh, Donghoon; Lee, Chang-Ha

2015-07-17

The effects of a malfunctional column on the performance of a simulated moving bed (SMB) process were studied experimentally and theoretically. The experimental results of conventional four-zone SMB (2-2-2-2 configuration) and FeedCol operation (2-2-2-2 configuration with one feed column) with one malfunctional column were compared with simulation results of the corresponding SMB processes with a normal column configuration. The malfunctional column in SMB processes significantly deteriorated raffinate purity. However, the extract purity was equivalent or slightly improved compared with the corresponding normal SMB operation because the complete separation zone of the malfunctional column moved to a lower flow rate range in zones II and III. With the malfunctional column configuration, FeedCol operation gave better experimental performance (up to 7%) than conventional SMB operation because controlling product purity with FeedCol operation was more flexible through the use of two additional operating variables, injection time and injection length. Thus, compared with conventional SMB separation, extract with equivalent or slightly better purity could be produced from FeedCol operation even with a malfunctional column, while minimizing the decrease in raffinate purity (less than 2%). Copyright © 2015 Elsevier B.V. All rights reserved.

Ionization of Xenon to the Nickel-Like Stage and Beyond in Micro-Capillary Plasma Columns Heated by Ultrafast Current Pulses

NASA Astrophysics Data System (ADS)

Avaria, G.; Grisham, M.; Li, J.; Tomasel, F. G.; Shlyapstsev, V. N.; Busquet, M.; Woolston, M.; Rocca, J. J.

Homogeneous plasma columns with ionization levels typical of MA discharges were created by rapidly heating gas-filled 520 µm diameter channels with ns rise-time current pulses of unusually low amplitude, 40 kA. These conditions allow the generation of high aspect ratio (eg. > 300:1) plasma columns with very high degrees of ionization (e.g. Ni-like Xenon) of interest for soft x-ray lasers below λ = 10 nm. Spectra and simulations of plasmas generated in 520 µm diameter alumina capillaries driven by 35-40 kA current pulses with 4 ns rise time were obtained for discharges in Xenon and Neon discharges. The first shows the presence of lines corresponding to ionization stages up to Fe-like Xe. The latter show that Al impurities from the walls are ionized to the H-like and He-like stages. He-like Al spectra containing the resonance line significantly broaden by opacity, the intercombination line, and Li-like satellites are analyzed. For Xenon discharges, the spectral lines from the Ni-like transitions the 3d94d (3/2, 3/2)J = 0 to the 3d94p(5/2, 3/2)J = 1 and to 3d94p(3/2, 1/2)J = 1 are observed.

Extraction and preparation of high-aroma and low-caffeine instant green teas by the novel column chromatographic extraction method with gradient elution.

PubMed

Li, Qing-Rong; Wu, Min; Huang, Rui-Jie; Chen, Ya-Fei; Chen, Chan-Jian; Li, Hui; Ni, He; Li, Hai-Hang

2017-06-01

The lack of aroma and natural taste is a critical problem in production and consumption of instant green teas. A method to prepare instant green teas high in-natural-aroma and low-caffeine by the novel column chromatographic extraction with gradient elution is reported. This method simultaneously extracted aroma (or volatile) and non-aroma compounds from green tea. Green tea was loaded into columns with 2.0-fold of petroleum ether (PE): ethanol (8:2). After standing for 3 h until the aroma compounds dissolved, the column was sequentially eluted with 3.0-fold 40% ethanol and 3.5-fold water. The eluant was collected together and automatically separated into PE and ethanol aqueous phases. The aroma extracts was obtained by vacuum-evaporation of PE phase at 45 °C. The ethanol aqueous phase was vacuum-concentrated to aqueous and partially or fully decaffeinated with 4% or 9% charcoal at 70 °C. A regular instant green tea with epigallocatechin-3-gallate: caffeine of 3.5:1 and a low-caffeine instant green tea (less than 1% caffeine) with excellent aroma and taste were prepared, by combining the aroma and non-aroma extracts at a 1:10 ratio. This work provides a practical approach to solve the low-aroma and low-taste problems in the production of high quality instant green teas.

Zinc oxide crystal whiskers as a novel sorbent for solid-phase extraction of flavonoids.

PubMed

Wang, Licheng; Shangguan, Yangnan; Hou, Xiudan; Jia, Yong; Liu, Shujuan; Sun, Yingxin; Guo, Yong

2017-08-15

As a novel solid-phase extraction material, zinc oxide crystal whiskers were used to extract flavonoid compounds and showed good extraction abilities. X-ray diffraction, scanning electron microscopy with energy dispersive X-ray spectroscopy and surface area/pore volume characterized the sorbent. The zinc oxide was packed into a solid-phase extraction micro-column and its extraction ability was evaluated by four model flavonoid compounds. The sample loading and elution parameters were optimized and the zinc oxide based analytical method for flavonoids was established. It showed that the method has wide linearities from 1 to 150μg/L and low limits of detection at 0.25μg/L. The relative standard deviations of a single column repeatability and column to column reproducibility were less than 6.8% and 10.6%. Several real samples were analyzed by the established method and satisfactory results were obtained. The interactions between flavonoids and zinc oxide were calculated and proved to be from the Van der Waals' forces between the 4p and 5d orbitals from zinc atom and the neighboring π orbitals from flavonoid phenyl groups. Moreover, the zinc oxide crystal whiskers showed good stability and could be reused more than 50 times under the operation conditions. This work proves that the zinc oxide crystal whiskers are a good candidate for flavonoids enrichment. Copyright © 2017. Published by Elsevier B.V.

Simultaneous separation and detection of actinides in acidic solutions using an extractive scintillating resin.

PubMed

Roane, J E; DeVol, T A

2002-11-01

An extractive scintillating resin was evaluated for the simultaneous separation and detection of actinides in acidic solutions. The transuranic extractive scintillating (TRU-ES) resin is composed of an inert macroporous polystyrene core impregnated with organic fluors (diphenyloxazole and 1,4-bis-(4-methyl-5-phenyl-2-oxazolyl)benzene) and an extractant (octyl(phenyl)-N,N-diisobutylcarbamoylmethylphosphine oxide in tributyl phosphate). The TRU-ES resin was packed into FEP Teflon tubing to produce a flow cell (0.2-mL free column volume), which is placed into a scintillation detection system to obtain pulse height spectra and time series data during loading and elution of actinides onto/from the resin. The alpha-particle absolute detection efficiencies ranged from 77% to 96.5%, depending on the alpha energy and quench. In addition to the on-line analyses, off-line analyses of the effluent can be conducted using conventional detection methods. The TRU-ES resin was applied to the quantification of a mixed radionuclide solution and two actual waste samples. The on-line characterization of the mixed radionuclide solution was within 10% of the reported activities whereas the agreement with the waste samples was not as good due to sorption onto the sample container walls and the oxidation state of plutonium. Agreement between the on-line and off-line analyses was within 35% of one another for both waste samples.

Effects of Monovalent and Divalent Salt Solutions on the Transport of Toxoplasma gondii in Saturated Porous Media

NASA Astrophysics Data System (ADS)

Darnault, C. J. G.; Pullano, C. P.; Mutty, T.; L'Ollivier, C.; Dubey, J. P.; Dumetre, A.

2017-12-01

The pathogenic microorganism Toxoplasma gondii is a current public health threat. Knowledge of the fate and transport of T. gondii in the environment, especially the subsurface, is critical to evaluate the risk of soil and groundwater contaminations. The physico-chemcial properties of groundwater systems, i.e. solution chemistry and aquifer materials, play a key role in the interaction of biocolloids with surfaces and therefore their mobility. This research examines how different salt solutions alter the mobility of T. gondii through saturated porous media. Salt solutions containing varying ionic strengths and concentrations of sodium chloride, calcium chloride, and magnesium chloride were used to test the transport of the T. gondii oocysts. These tests were performed using quartz silica sand columns fed by a peristaltic pump in order to generate flow and transport of the biocolloids. The salt solution was pumped though the column followed by a pulse of the T. gondii oocysts, then a pulse of salt solution without oocysts, and then lastly a pulse of distilled water. Sampling of the solution exiting the columns was tested for T. gondii oocysts using qPCR in order to quantify the oocysts present. The breakthough curve results were then compared to a conservative bromide tracer test in order to determine the factors associated with the movement of these biocolloids through the sand columns. A model of the flow of the toxoplasma colloids through the sand matrix was made in order to characterize the parameters affecting the transport and retention of T. gondii occysts though saturated porous media.

[Preparation and applications of a supported liquid-liquid extraction column with a composite diatomite material].

PubMed

Bao, Jianmin; Ma, Zhishuang; Sun, Ying; Wang, Yongzun; Li, Youxin

2012-08-01

A rapid and special supported liquid-liquid extraction (SLE) column was developed with a composite diatomite material. The SLE column was evaluated by high performance liquid chromatography (HPLC) with acidic, neutral and alkaline compounds dissolved in water. Furthermore, some real complex samples were also analyzed by HPLC with the SLE method. The recoveries of benzoic acid (acidic), p-nitroaniline (alkaline) and 4-hydroxy-benzoic methyl ester (neutral) treated by the SLE column were 90.6%, 98.1% and 97.7%. However, the recoveries of the three compounds treated by traditional liquid-liquid extraction (LLE) method were 71.9%, 81.9% and 83.9%. The results showed that the SLE technique had higher recoveries than the traditional LLE method. The spiked recoveries of the complex samples, such as benzoic acid in Sprite and dexamethasone acetate, chlorphenamine maleate, indomethacin in bovine serum, were between 80% and 110% and the relative standard deviations (RSDs) were less than 15%. For biological specimen, the results could be accepted. Meantime, many disadvantages associated with traditional LLE method, such as emulsion formation, didn't occur using SLE column. The SLE column technique is a good sample preparation method with many advantages, such as rapid, simple, robust, easily automated, high recovery and high-throughput, which would be widely used in the future.

Semi-permeable surface analytical reversed-phase column for the improved trace analysis of acidic pesticides in water with coupled-column reversed-phase liquid chromatography with UV detection. Determination of bromoxynil and bentazone in surface water.

PubMed

Hogendoorn, E A; Westhuis, K; Dijkman, E; Heusinkveld, H A; den Boer, A C; Evers, E A; Baumann, R A

1999-10-08

The coupled-column (LC-LC) configuration consisting of a 3 microm C18 column (50 x 4.6 mm I.D.) as the first column and a 5 microm C18 semi-permeable-surface (SPS) column (150 x 4.6 mm I.D.) as the second column appeared to be successful for the screening of acidic pesticides in surface water samples. In comparison to LC-LC employing two C18 columns, the combination of C18/SPS-C18 significantly decreased the baseline deviation caused by the hump of the co-extracted humic substances when using UV detection (217 nm). The developed LC-LC procedure allowed the simultaneous determination of the target analytes bentazone and bromoxynil in uncleaned extracts of surface water samples to a level of 0.05 microg/l in less than 15 min. In combination with a simple solid-phase extraction step (200 ml of water on a 500 mg C18-bonded silica) the analytical procedure provides a high sample throughput. During a period of about five months more than 200 ditch-water samples originating from agricultural locations were analyzed with the developed procedure. Validation of the method was performed by randomly analyzing recoveries of water samples spiked at levels of 0.1 microg/l (n=10), 0.5 microg/l (n=7) and 2.5 microg/l (n=4). Weighted regression of the recovery data showed that the method provides overall recoveries of 95 and 100% for bentazone and bromoxynil, respectively, with corresponding intra-laboratory reproducibilities of 10 and 11%, respectively. Confirmation of the analytes in part of the samples extracts was carried out with GC-negative ion chemical ionization MS involving a derivatization step with bis(trifluoromethyl)benzyl bromide. No false negatives or positives were observed.

Structures of the Oligosaccharides of the Glycoprotein Coded by Early Region E3 of Adenovirus 2

PubMed Central

Kornfeld, Rosalind; Wold, William S. M.

1981-01-01

Early region E3 of adenovirus 2 encodes a glycoprotein, E3-gp25K, that is a good model with which to study structure-function relationships in transmembrane glycoproteins. We have determined the structures of the oligosaccharides linked to E3-gp25K. The oligosaccharides were labeled with [2-3H]mannose in adenovirus 2-early infected KB cells for 5.5h (pulse) or for 5.5 h followed by a 3-h chase (pulse-chase). E3-gp25K was extracted and purified by chromatography on DEAE-Sephacel in 7 M urea, followed by gel filtration on a column of Bio-Gel A-1.5m in 6 M guanidine hydrochloride. An analysis of the purified protein by sodium dodecyl sulfate-polyacrylamide gel electrophoresis indicated that it was >95% pure. The oligosaccharides were isolated by pronase digestion followed by gel filtration on a column of Bio-Gel P-6, then by digestion with endo-β-N-acetylglucosaminidase H, followed by gel filtration on Bio-Gel P-6, and finally by paper chromatography. The pulse sample contained equal amounts of Man9GlcNAc and Man8GlcNAc and small amounts of Man7GlcNAc and Man6GlcNAc. The pulse-chase sample had predominantly Man8GlcNAc and much less Man9GlcNAc, indicating that processing of the Man9GlcNAc to Man8GlcNAc had occurred during the chase period. Thus, Man8GlcNAc is the major oligosaccharide on mature E3-gp25K. The structures of these oligosaccharides were established by digestion with α-mannosidase, methylation analysis, and acetolysis. The oligosaccharides found had typical high-mannose structures that have been observed in other membrane and soluble glycoproteins, and the branching patterns and linkages of the mannose residues of Man9GlcNAc were identical to those of the lipid-linked Glc3Man9GlcNAc2 donor. Thus, adenovirus 2 infection (early stages) apparently does not affect the usual cellular high-mannose glycosylation pathways, and despite being virus coded, E3-gp25K is glycosylated in the same manner as a typical mammalian cell-coded glycoprotein. Images PMID:7321093

Structures of the oligosaccharides of the glycoprotein coded by early region E3 of adenovirus 2.

PubMed

Kornfeld, R; Wold, W S

1981-11-01

Early region E3 of adenovirus 2 encodes a glycoprotein, E3-gp25K, that is a good model with which to study structure-function relationships in transmembrane glycoproteins. We have determined the structures of the oligosaccharides linked to E3-gp25K. The oligosaccharides were labeled with [2-(3)H]mannose in adenovirus 2-early infected KB cells for 5.5h (pulse) or for 5.5 h followed by a 3-h chase (pulse-chase). E3-gp25K was extracted and purified by chromatography on DEAE-Sephacel in 7 M urea, followed by gel filtration on a column of Bio-Gel A-1.5m in 6 M guanidine hydrochloride. An analysis of the purified protein by sodium dodecyl sulfate-polyacrylamide gel electrophoresis indicated that it was >95% pure. The oligosaccharides were isolated by pronase digestion followed by gel filtration on a column of Bio-Gel P-6, then by digestion with endo-beta-N-acetylglucosaminidase H, followed by gel filtration on Bio-Gel P-6, and finally by paper chromatography. The pulse sample contained equal amounts of Man(9)GlcNAc and Man(8)GlcNAc and small amounts of Man(7)GlcNAc and Man(6)GlcNAc. The pulse-chase sample had predominantly Man(8)GlcNAc and much less Man(9)GlcNAc, indicating that processing of the Man(9)GlcNAc to Man(8)GlcNAc had occurred during the chase period. Thus, Man(8)GlcNAc is the major oligosaccharide on mature E3-gp25K. The structures of these oligosaccharides were established by digestion with alpha-mannosidase, methylation analysis, and acetolysis. The oligosaccharides found had typical high-mannose structures that have been observed in other membrane and soluble glycoproteins, and the branching patterns and linkages of the mannose residues of Man(9)GlcNAc were identical to those of the lipid-linked Glc(3)Man(9)GlcNAc(2) donor. Thus, adenovirus 2 infection (early stages) apparently does not affect the usual cellular high-mannose glycosylation pathways, and despite being virus coded, E3-gp25K is glycosylated in the same manner as a typical mammalian cell-coded glycoprotein.

Hexahedral finite element mesh coarsening using pillowing technique

DOEpatents

Staten, Matthew L [Pittsburgh, PA; Woodbury, Adam C [Provo, UT; Benzley, Steven E [Provo, UT; Shepherd, Jason F [Edgewood, NM

2012-06-05

A techniques for coarsening a hexahedral mesh is described. The technique includes identifying a coarsening region within a hexahedral mesh to be coarsened. A boundary sheet of hexahedral elements is inserted into the hexahedral mesh around the coarsening region. A column of hexahedral elements is identified within the boundary sheet. The column of hexahedral elements is collapsed to create an extraction sheet of hexahedral elements contained within the coarsening region. Then, the extraction sheet of hexahedral elements is extracted to coarsen the hexahedral mesh.

An on-line coupling of nanofibrous extraction with column-switching high performance liquid chromatography - A case study on the determination of bisphenol A in environmental water samples.

PubMed

Háková, Martina; Chocholoušová Havlíková, Lucie; Chvojka, Jiří; Solich, Petr; Šatínský, Dalibor

2018-02-01

Polyamide 6 nanofiber polymers were used as modern sorbents for on-line solid phase extraction (SPE) coupled with liquid chromatography. The on-line SPE system was tested for the determination of bisphenol A in river water samples. Polyamide nanofibers were prepared using needleless electrospinning, inserted into a mini-column cartridge (5 × 4.6mm) and coupled with HPLC. The effect of column packing and the amount of polyamide 6 on extraction efficiency was tested and the packing process was optimized. The proposed method was performed using a 50-µL sample injection followed by an on-line nanofibrous extraction procedure. The influence of the washing mobile phase on the retention of bisphenol A during the extraction procedure was evaluated. Ascentis ® Express C18 (10cm × 4.6mm) core-shell column was used as an analytical column. Fluorescence detection wavelengths (λ ex = 225nm and λ em = 320nm) were used for identification and quantification of Bisphenol A in river waters. The linearity was tested in the range from 2 to 500µgL -1 (using nine calibration points). The limits of detection and quantification were 0.6 and 2µgL -1 , respectively. The developed method was successfully used for the determination of bisphenol A in various samples of river waters in the Czech Republic (The Ohře, Labe, Nisa, Úpa, and Opava Rivers). Copyright © 2017 Elsevier B.V. All rights reserved.

Electric field controlled emulsion phase contactor

DOEpatents

Scott, Timothy C.

1995-01-01

A system for contacting liquid phases comprising a column for transporting a liquid phase contacting system, the column having upper and lower regions. The upper region has a nozzle for introducing a dispersed phase and means for applying thereto a vertically oriented high intensity pulsed electric field. This electric field allows improved flow rates while shattering the dispersed phase into many micro-droplets upon exiting the nozzle to form a dispersion within a continuous phase. The lower region employs means for applying to the dispersed phase a horizontally oriented high intensity pulsed electric field so that the dispersed phase undergoes continuous coalescence and redispersion while being urged from side to side as it progresses through the system, increasing greatly the mass transfer opportunity.

Method of using an electric field controlled emulsion phase contactor

DOEpatents

Scott, Timothy C.

1993-01-01

A system for contacting liquid phases comprising a column for transporting a liquid phase contacting system, the column having upper and lower regions. The upper region has a nozzle for introducing a dispersed phase and means for applying thereto a vertically oriented high intensity pulsed electric field. This electric field allows improved flow rates while shattering the dispersed phase into many micro-droplets upon exiting the nozzle to form a dispersion within a continuous phase. The lower region employs means for applying to the dispersed phase a horizontally oriented high intensity pulsed electric field so that the dispersed phase undergoes continuous coalescence and redispersion while being urged from side to side as it progresses through the system, increasing greatly the mass transfer opportunity.

Electric field controlled emulsion phase contactor

DOEpatents

Scott, T.C.

1995-01-31

A system is described for contacting liquid phases comprising a column for transporting a liquid phase contacting system, the column having upper and lower regions. The upper region has a nozzle for introducing a dispersed phase and means for applying thereto a vertically oriented high intensity pulsed electric field. This electric field allows improved flow rates while shattering the dispersed phase into many micro-droplets upon exiting the nozzle to form a dispersion within a continuous phase. The lower region employs means for applying to the dispersed phase a horizontally oriented high intensity pulsed electric field so that the dispersed phase undergoes continuous coalescence and redispersion while being urged from side to side as it progresses through the system, increasing greatly the mass transfer opportunity. 5 figs.

Langmuir probe measurements of double-layers in a pulsed discharge

NASA Technical Reports Server (NTRS)

Levine, J. S.; Crawford, F. W.

1980-01-01

Langmuir probe measurements were carried out which confirm the occurrence of double-layers in an argon positive column. Pulsing the discharge current permitted probe measurements to be performed in the presence of the double-layer. Supplementary evidence, obtained from DC and pulsed discharges, indicated that the double-layers formed in the two modes of operation were similar. The double-layers observed were weak and stable; their relation to other classes of double-layers are discussed, and directions for future work are suggested.

Development of andrographolide molecularly imprinted polymer for solid-phase extraction

NASA Astrophysics Data System (ADS)

Yin, Xiaoying; Liu, Qingshan; Jiang, Yifan; Luo, Yongming

2011-06-01

A method employing molecularly imprinted polymer (MIP) as selective sorbent for solid-phase extraction (SPE) to pretreat samples was developed. The polymers were prepared by precipitation polymerization with andrographolide as template molecule. The structure of MIP was characterized and its static adsorption capacity was measured by the Scatchard equation. In comparison with C 18-SPE and non-imprinted polymer (NIP) SPE column, MIP-SPE column displays high selectivity and good affinity for andrographolide and dehydroandrographolide for extract of herb Andrographis paniculata ( Burm.f.) Nees (APN). MIP-SPE column capacity was 11.9 ± 0.6 μmol/g and 12.1 ± 0.5 μmol/g for andrographolide and dehydroandrographolide, respectively and was 2-3 times higher than that of other two columns. The precision and accuracy of the method developed were satisfactory with recoveries between 96.4% and 103.8% (RSD 3.1-4.3%, n = 5) and 96.0% and 104.2% (RSD 2.9-3.7%, n = 5) for andrographolide and dehydroandrographolide, respectively. Various real samples were employed to confirm the feasibility of method. This developed method demonstrates the potential of molecularly imprinted solid phase extraction for rapid, selective, and effective sample pretreatment.

Combined extraction-cleanup column chromatographic procedure for determination of dicofol in avian eggs

USGS Publications Warehouse

Krynitsky, A.J.; Stafford, C.J.; Wiemeyer, Stanley N.

1988-01-01

Dicofol in avian eggs was completely oxidized to dichlorobenzophenone (DCBP) when a hexane Soxhlet extraction procedure was used. This degradation did not occur with other avian tissues (muscle and liver). For this reason, a combined extraction-cleanup column chromatographic procedure, without added heat, was developed for the determination of dicofol in avian eggs. Homogenized subsamples of eggs were mixed with sodium sulfate, and the mixture was added as the top layer on a column prepacked with Florisil. The dicofol and other compounds of interest were then eluted with ethyl ether-hexane. The extracts, relatively free from lipids, were quantitated on a gas chromatograph equipped with a 63Ni electron-capture detector and a methyl silicone capillary column. Recoveries from chicken eggs, fortified with dicofol and other DDT-related compounds, averaged 96%. Analysis of eggs of eastern screech-owls, fed a meat diet containing 10 ppm technical Kelthane, showed that both dicofol and DCBP were present. Results were confirmed by gas chromatography/mass spectrometry. This method is rapid and reliable, involves a minimum of sample handling, and is well suited for high volume determination of dicofol in eggs and other avian tissues.

A hybrid monolithic column based on boronate-functionalized graphene oxide nanosheets for online specific enrichment of glycoproteins.

PubMed

Zhou, Chanyuan; Chen, Xiaoman; Du, Zhuo; Li, Gongke; Xiao, Xiaohua; Cai, Zongwei

2017-05-19

A hybrid monolithic column based on aminophenylboronic acid (APBA)-functionalized graphene oxide (GO) has been developed and used for selective enrichment of glycoproteins. The APBA/GO composites were homogeneously incorporated into a polymer monolithic column with the help of oligomer matrix and followed by in situ polymerization. The effect of dispersion of APBA/GO composites in the polymerization mixture on the performance of the monolithic column was explored in detail. The presence of graphene oxide not only enlarged the BET surface area from 6.3m 2 /g to 169.4m 2 /g, but also provided abundant boronic acid moieties for glycoprotein extraction, which improved the enrichment selectivity and efficiency for glycoproteins. The APBA/GO hybrid monolithic column was incorporated into a sequential injection system, which facilitated online extraction of proteins. Combining the superior properties of extraordinary surface area of GO and the affinity interaction of APBA to glycoproteins, the APBA/GO hybrid monolithic column showed higher enrichment factors for glycoproteins than other proteins without cis-diol-containing groups. Also, under comparable or even shorter processing time and without the addition of any organic solvent, it showed higher binding capacity toward glycoproteins compared with the conventional boronate affinity monolithic column. The practical applicability of this system was demonstrated by processing of egg white samples for extraction of ovalbumin and ovotransferrin, and satisfactory results were obtained by assay with SDS-PAGE. Copyright © 2017 Elsevier B.V. All rights reserved.

Phyto (in)stabilization of elements.

PubMed

Jacob, Donna L; Otte, Marinus L; Hopkins, David G

2011-01-01

The effects of plants (corn, soybean, and sunflower) and fertilizer on mobility of more than 60 elements were assessed in a greenhouse experiment. Unplanted columns with the same soil served as controls. Half the columns received fertilizer and all columns were watered at the same rate. At the end of the experiment, the columns were watered to mimic a rainstorm event such that water drained from the bases of the columns, which was collected and analyzed for element content. Soil from between the roots of the plants was also collected and the water-extractable fraction determined. It was expected that (1) more mobile elements, as measured by water extraction, would be leached from the soils at a higher rate compared to less mobile elements, (2) plants would immobilize most elements, but that some would be immobilized, and (3) that this would depend on plant species. The results led to the following conclusions: plants cause metal mobility to vary over a wide range for a specific soil and do mobilize some elements (e.g., Th) while immobilizing others (e.g., U). The effects depended on plant species for some elements. Water-extractable fractions of elements do not predict mobility.

Guiding of laser pulses in plasma waveguides created by linearly-polarized femtosecond laser pulses

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

Lemos, N.; Cardoso, L.; Geada, J.

We experimentally demonstrate that plasma waveguides produced with ultra-short laser pulses (sub-picosecond) in gas jets are capable of guiding high intensity laser pulses. This scheme has the unique ability of guiding a high-intensity laser pulse in a plasma waveguide created by the same laser system in the very simple and stable experimental setup. A hot plasma column was created by a femtosecond class laser that expands into an on-axis parabolic low density profile suitable to act as a waveguide for high intensity laser beams. We have successfully guided ~10 15 W cm -2 laser pulses in a 8 mm longmore » hydrogen plasma waveguide with a 35% guiding efficiency.« less

Guiding of laser pulses in plasma waveguides created by linearly-polarized femtosecond laser pulses

DOE PAGES

Lemos, N.; Cardoso, L.; Geada, J.; ...

2018-02-16

We experimentally demonstrate that plasma waveguides produced with ultra-short laser pulses (sub-picosecond) in gas jets are capable of guiding high intensity laser pulses. This scheme has the unique ability of guiding a high-intensity laser pulse in a plasma waveguide created by the same laser system in the very simple and stable experimental setup. A hot plasma column was created by a femtosecond class laser that expands into an on-axis parabolic low density profile suitable to act as a waveguide for high intensity laser beams. We have successfully guided ~10 15 W cm -2 laser pulses in a 8 mm longmore » hydrogen plasma waveguide with a 35% guiding efficiency.« less

Determination of Total Biotin by Liquid Chromatography Coupled with Immunoaffinity Column Cleanup Extraction: Multilaboratory Testing, Final Action 2016.02.

PubMed

Joseph, George; Devi, Ranjani; Marley, Elaine C; Leeman, David

2018-05-01

Single- and multilaboratory testing data have provided systematic scientific evidence that a simple, selective, accurate, and precise method can be used as a potential candidate reference method for dispute resolution in determining total biotin in all forms of infant, adult, and/or pediatric formula. Using LC coupled with immunoaffinity column cleanup extraction, the method fully meets the intended purpose and applicability statement in AOAC Standard Method Performance Requirement 2014.005. The method was applied to a cross-section of infant formula and adult nutritional matrixes, and acceptable precision and accuracy were established. The analytical platform is inexpensive, and the method can be used in almost any laboratory worldwide with basic facilities. The immunoaffinity column cleanup extraction is the key step to successful analysis.

Application of mercapto-silica polymerized high internal phase emulsions for the solid-phase extraction and preconcentration of trace lead(II).

PubMed

Su, Rihui; Ruan, Guihua; Chen, Zhengyi; Du, Fuyou; Li, Jianping

2015-12-01

A new class of solid-phase extraction column prepared with grafted mercapto-silica polymerized high internal phase emulsion particles was used for the preconcentration of trace lead. First, mercapto-silica polymerized high internal phase emulsion particles were synthesized by using high internal phase emulsion polymerization and carefully assembled in a polyethylene syringe column. The influences of various parameters including adsorption pH value, adsorption and desorption solvents, flow rate of the adsorption and desorption procedure were optimized, respectively, and the suitable uploading sample volumes, adsorption capacity, and reusability of solid phase extraction column were also investigated. Under the optimum conditions, Pb(2+) could be preconcentrated quantitatively over a wide pH range (2.0-5.0). In the presence of foreign ions, such as Na(+) , K(+) , Ca(2+) , Zn(2+) , Mg(2+) , Cu(2+) , Fe(2+) , Cd(2+) , Cl(-) and NO3 (-) , Pb(2+) could be recovered successfully. The prepared solid-phase extraction column performed with high stability and desirable durability, which allowed more than 100 replicate extractions without measurable changes of performance. The feasibility of the developed method was further validated by the extraction of Pb(2+) in rice samples. At three spiked levels of 40.0, 200 and 800 μg/kg, the average recoveries for Pb(2+) in rice samples ranged from 87.3 to 105.2%. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Comparison of twin-cell centrifugal partition chromatographic columns with different cell volume.

PubMed

Goll, Johannes; Audo, Gregoire; Minceva, Mirjana

2015-08-07

Two twin-cell centrifugal partition chromatographic columns (SCPC 250 and SCPE-250-BIO, Armen Instrument, France) with the same column volume but different cell size and number were compared in terms of stationary phase retention and column efficiency. The columns were tested with two types of solvent systems: a commonly used organic solvent based biphasic system from the ARIZONA solvent system family and a polymer/salt based aqueous two phase system (ATPS). The efficiency of the columns was evaluated by pulse injection experiments of two benzenediols (pyrocatechol and hydroquinone) in the case of the ARIZONA system and a protein mixture (myoglobin and lysozyme) in the case of the ATPS. As result of high stationary phase retention, the column with the lower number of larger twin-cells (SCPE-250-BIO) is suitable for protein separations using ATPS. On the other hand, due to higher column efficiency, the column with the greater number of smaller cells (SCPC 250) is superior for batch elution separations performed with standard liquid-liquid chromatography organic solvent based biphasic systems. Copyright © 2015 Elsevier B.V. All rights reserved.

[Immunoaffinity columns and determination of ochratoxin A in cereals by HPLC. Part I.: Evaluation of extraction using methanol/water].

PubMed

Czerwiecki, Ludwik; Czyzyk, Kamila; Kwiecień, Agnieszka; Wilczyńska, Grazyna

2004-01-01

The method for ochratoxin A determination in cereals (wheat, rye) was described. Application of immunoaffinity columns (IAC) for clean-up of extracts was investigated. The ochratoxin A content was determined by high-performance liquid chromatography using C18 column and fluorimetric detection at 330 nm (excitation) and 460 nm (emission). The mean recovery of ochratoxin A was 65-78%. The limits of detection (LOD) and quantification (LOQ) were 0.015 and 0.025 microg/kg, respectively. The positive results were confirmed by reaction with BF3 complex in methanol.

[Determination of deoxynivalenol in grain and its products by solid-phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry].

PubMed

Huang, Juan; Chen, Guosong; Zhang, Xiaoyan; Shen, Chongyu; Lü, Chen; Wu, Bin; Liu, Yan; Chen, Huilan; Ding, Tao

2012-11-01

A method was established for the determination of deoxynivalenol (vomitoxin) in grain and its products based on solid-phase extraction coupled with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The sample was firstly extracted by acetonitrile-water (84:16, v/v). The extract was then cleaned-up by an HLB solid phase extraction cartridge. The separation was carried out on a Phenomenex Kinetex C18 column (100 mm x4. 6 mm, 2.6 microm) with a gradient elution using 0.3% per hundred ammonia solution-acetonitrile as mobile phases. The analysis of deoxynivalenol was performed under electrospray negative ionization mode. The limit of detection (LOD, S/N= 3) and the limit of quantification (LOQ, S/N = 10) were 20 microg/kg and 50 microg/kg, respectively. A good linearity (r > 0.99) was achieved for the target compound over the range of 20-1000 pg/L. The recoveries at the three spiked levels (50, 100, 500 microg/kg) in the blank matrices such as flour, barley, soybean, rice, cornmeal, cassava and wheat, were varied from 75.6% to 111.0% with the relative standard deviations no more than 13. 0%. The method is accurate, efficient, sensitive and practical. The cost of pretreatment is obviously reduced by replacing immunoaffinity columns and Mycosep columns with HLB columns which have the same purification effect.

Multi-mJ energy extraction using Yb-fiber based coherent pulse stacking amplification of fs pulses (Conference Presentation)

NASA Astrophysics Data System (ADS)

Ruppe, John M.; Pei, Hanzhang; Chen, Siyun; Sheikhsofla, Morteza; Wilcox, Russell B.; Nees, John A.; Galvanauskas, Almantas

2017-03-01

We report multi-mJ energy (>5mJ) extraction from femtosecond-pulse Yb-doped fiber CPA using coherent pulse stacking amplification (CPSA) technique. This high energy extraction has been enabled by amplifying 10's of nanosecond long pulse sequence, and by using 85-µm core Yb-doped CCC fiber based power amplification stage. The CPSA system consists of 1-GHz repetition rate mode-locked fiber oscillator, followed by a pair of fast phase and amplitude electro-optic modulators, a diffraction-grating based pulse stretcher, a fiber amplifier chain, a GTI-cavity based pulse stacker, and a diffraction grating pulse compressor. Electro-optic modulators are used to carve out from the 1-GHz mode-locked pulse train an amplitude and phase modulated pulse burst, which after stretching and amplification, becomes equal-amplitude pulse burst consisting of 27 stretched pulses, each approximately 1-ns long. Initial pulse-burst shaping accounts for the strong amplifier saturation effects, so that it is compensated at the power amplifier output. This 27-pulse burst is then coherently stacked into a single pulse using a multiplexed sequence of 5 GTI cavities. The compact-footprint 4+1 multiplexed pulse stacker consists of 4 cavities having rountrip of 1 ns, and one Herriott-cell folded cavity - with 9ns roundtrip. After stacking, stretched pulses are compressed down to the bandwidth-limited 300 fs duration using a standard diffraction-grating pulse compressor.

[Poetry Instruction.] Motivator of the Month. [Compiled from Columns in Three issues of "Notes Plus," January and November 1984 and September 1985.

ERIC Educational Resources Information Center

Notes Plus, 1985

1985-01-01

The teaching activities presented in the four journal columns extracted here focus on understanding and writing poetry. The first column (by Carol Case) presents an introduction to poetry unit containing five preliminary steps designed to help students develop an understanding of poetry. The second column (by Carol Anderson) describes a week of…

Separation of the Components of a Commercial Analgesic Tablet: A Two-Week Sequence Comparing Purification by Two-Base Extraction and Column Chromatography

ERIC Educational Resources Information Center

Revell, Kevin D.

2011-01-01

A new laboratory experiment is described in which students compare two benchtop separation methods to isolate the three active components of the commercial analgesic Excedrin. In the two-week sequence, aspirin, acetaminophen, and caffeine are separated using either a two-base liquid-liquid extraction or silica column chromatography. Students then…

An on-line SPE-HPLC method for effective sample preconcentration and determination of fenoxycarb and cis, trans-permethrin in surface waters.

PubMed

Šatínský, Dalibor; Naibrtová, Linda; Fernández-Ramos, Carolina; Solich, Petr

2015-09-01

A new on-line SPE-HPLC method using fused-core columns for on-line solid phase extraction and large volume sample injection for increasing the sensitivity of detection was developed for the determination of insecticides fenoxycarb and cis-, trans-permethrin in surface waters. The separation was carried out on fused-core column Phenyl-Hexyl (100×4.6 mm), particle size 2.7 µm with mobile phase acetonitrile:water in gradient mode at flow rate 1.0 mL min(-1), column temperature 45°C. Large volume sample injection (1500 µL) to the extraction dimension using short precolumn Ascentis Express RP C-18 (5×4.6 mm); fused-core particle size 2.7 µm allowed effective sample preconcentration and efficient ballast sample matrix removal. The washing mobile phase consisting of a mixture of acetonitrile:water; 30:70, (v/v) was pumped at flow rate of 0.5 mL min(-1) through the extraction precolumn to the waste. Time of the valve switch for transferring the preconcentrated sample zone from the extraction to the separation column was set at 3rd min. Elution of preconcentrated insecticides from the extraction precolumn and separation on the analytical column was performed in gradient mode. Linear gradient elution started from 40% of acetonitrile at time of valve switch from SPE column (3rd min) to 95% of acetonitrile at 7th min. Synthetic dye sudan I was chosen as an internal standard. UV detection at wavelength 225 nm was used and the method reached the limits of detection (LOD) at ng mL(-1) levels for both insecticides. The method showing on-line sample pretreatment and preconcentration with highly sensitive determination of insecticides was applied for monitoring of fenoxycarb and both permethrin isomers in different surface water samples in Czech Republic. The time of whole analysis including on-line extraction, interferences removal, chromatography separation and system equilibration was less than 8 min. Copyright © 2015 Elsevier B.V. All rights reserved.

Re-evaluation of solid-phase adsorption and desorption techniques for isolation of trace organic pollutants from chlorinated water.

PubMed

Onodera, S; Nagatsuka, A; Rokuhara, T; Asakura, T; Hirayama, N; Suzuki, S

1993-07-16

Amberlite XAD resin and activated carbon columns were tested for their abilities to concentrate trace organic pollutants in chlorinated water. Both XAD-2 and XAD-7 resin columns (20 ml) were capable of adsorbing about 30% of total organic halogen (TOX) present in 20 l of drinking water (pH 7) containing about 100 micrograms/l of TOX, whereas the carbon column (10 ml) adsorbed over 90% of TOX. The adsorption capacity of XAD-7 resin was found to be strongly dependent on the solution pH, as compared with those of XAD-2 and carbon adsorbents. Soxhlet and sonication extractions were also evaluated for their abilities to recover the adsorbed organics from the adsorbents, by measurements of TOX, chromatographable compounds and mutagenicity in the eluates. Soxhlet extraction gave higher recoveries than sonication, as measured with the above indices, but these differences were generally small (ca. 20%), with exception of the carbon extracts. The XAD-2 and XAD-7 extracts of drinking water also showed about 3-4 times higher mutagenic activity than the carbon extracts.

Evidence for Pulsar-like Emission Components in the Broadband ULX Sample

NASA Astrophysics Data System (ADS)

Walton, D. J.; Fürst, F.; Heida, M.; Harrison, F. A.; Barret, D.; Stern, D.; Bachetti, M.; Brightman, M.; Fabian, A. C.; Middleton, M. J.

2018-04-01

We present broadband X-ray analyses of a sample of bright ultraluminous X-ray sources (ULX) with the goal of investigating the spectral similarity of this population to the known ULX pulsars, M82 X-2, NGC 7793 P13, and NGC 5907 ULX. We perform a phase-resolved analysis of the broadband XMM-Newton+NuSTAR data set of NGC 5907 ULX, finding that the pulsed emission from the accretion column in this source exhibits a similar spectral shape to that seen in both M82 X-2 and NGC 7793 P13, and that this is responsible for the excess emission observed at the highest energies when the spectra are fit with accretion disk models. We then demonstrate that similar “hard” excesses are seen in all ULXs in the broadband sample. Finally, for ULXs where the nature of the accretor is currently unknown, we test whether the hard excesses are all consistent with being produced by an accretion column similar to those present in M82 X-2, NGC 7793 P13, and NGC 5907 ULX. Based on the average shape of the pulsed emission, we find that in all cases a similar accretion column can successfully reproduce the observed data, consistent with the hypothesis that this ULX sample may be dominated by neutron star accretors. Compared to the known pulsar ULXs, our spectral fits for the remaining ULXs suggest that the non-pulsed emission from the accretion flow beyond the magnetosphere makes a stronger relative contribution than the component associated with the accretion column. If these sources do also contain neutron star accretors, this may help to explain the lack of detected pulsations.

Ion mobility based on column leaching of South African gold tailings dam with chemometric evaluation.

PubMed

Cukrowska, Ewa M; Govender, Koovila; Viljoen, Morris

2004-07-01

New column leaching experiments were designed and used as an alternative rapid screening approach to element mobility assessment. In these experiments, field-moist material was treated with an extracting solution to assess the effects of acidification on element mobility in mine tailings. The main advantage of this version of column leaching experiments with partitioned segments is that they give quick information on current element mobility in conditions closely simulating field conditions to compare with common unrepresentative air-dried, sieved samples used for column leaching experiments. Layers from the tailings dump material were sampled and packed into columns. The design of columns allows extracting leachates from each layer. The extracting solutions used were natural (pH 6.8) and acidified (pH 4.2) rainwater. Metals and anions were determined in the leachates. The concentrations of metals (Ca, Mg, Fe, Mn, Al, Cr, Ni, Co, Zn, and Cu) in sample leachates were determined using ICP OES. The most important anions (NO3-, Cl-, and SO4(2)-) were determined using the closed system izotacophoresis ITP analyser. The chemical analytical data from tailings leaching and physico-chemical data from field measurements (including pH, conductivity, redox potential, temperature) were used for chemometric evaluation of element mobility. Principal factor analysis (PFA) was used to evaluate ions mobility from different layers of tailings dump arising from varied pH and redox conditions. It was found that the results from the partitioned column leaching illustrate much better complex processes of metals mobility from tailings dump than the total column. The chemometric data analysis (PFA) proofed the differences in the various layers leachability that are arising from physico-chemical processes due to chemical composition of tailings dump deposit. Copyright 2004 Elsevier Ltd.

Regenerated silica gel as stationary phase on vacuum column chromatography to purify temulawak's extracts

NASA Astrophysics Data System (ADS)

Cahyono, Bambang; Maduwu, Ratna Dewi; Widayat, Suzery, Meiny

2015-12-01

Commercial silica gel only used once by many researchers and affected high cost for purification process, also less support the green chemistry program. This research focused in regeneration silica gel that used purification of temulawak's extracts (Curcuma xanthorrhiza Roxb) by vacuum column chromatography. Sample extracts (contains 10.1195±0.5971% of curcuminoids) was purified by vacuum column chromatography (pressure: 45 kPa, column: 100mm on length and 16mm on diameter). Ethanol 96% and acetone were compared as eluent. The amount of solvent and yield of curcuminoids used as indicator purification. The silica gel was regenerated with heating in 600°C for 8 hours The silica gels were analyzed by IR spectroscopy and X-ray diffraction. Furthermore, regenerated silica gel was used as the stationary phase in vacuum column chromatography under the same conditions with the previous purification. All the purification experiments were performed in three repetitions. Based on regression equation, y=0.132x+0.0011 (r2=0.9997) the yield of curcuminoids on purified products using ethanol as the eluent was improved 4.26% (to 14.3724±0.5749%) and by acetone was improved 3,03% (to 13.1450 ±0.6318%). The IR spectrum of both silica gel showed the same vibration profile and also there were three crystallinity peaks missing on its X-ray diffraction. Regenerated silica gel has the same performance with new silica gel in purification of temulawak's extract: by ethanol has increased 4.08% (14.1947±0.7415%) and 2.93% (13.0447±0.4822) by acetone. In addition, all purification products showed similar TLC profiles. Purification using regenerated silica gel as the adsorbent on vacuum column chromatography has exactly same potential with the new silica gel.

Identification of nonvolatile coal derived products via chromatography coupled with on-line FTIR detection. Quarterly progress report, March 1-May 31, 1985. [C/sub 2/H/sub 2/ extracts of ground coal, coffee and paprika

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

Taylor, L.T.

Because it has been our goal to interface the supercritical fluid chromatograph with a Fourier transform infrared spectrometer we have initially chosen packed columns due to their increased sample capacities, and supercritical CO/sub 2/ because of its infrared transparency. This paper compares two sampling techniques that can be utilized in packed column supercritical fluid Chromatography (SFC). Traditional sample introduction is accomplished using an injector with a sample loop. The loop is filled with the appropriate amount of material, and subsequently inserted into the mobile phase path. In most cases the sample must be either dissolved or extracted into an appropriatemore » solvent for such sample introduction. Note that unlike HPLC, where the solvent can be the same as the mobile phase, traditional sampling with SFC must use a solvent that is very different from the mobile phase. As a result, solvent peaks are almost always present, especially with universal detectors like FTIR. An alternative method is described here whereby both extraction of the sample and introduction of the extract onto the column is accomplished on-line using only the supercritical fluid mobile phase. This sampling technique is made possible by a simple valving scheme which ties directly the extraction vessel, the injector, the packed column and the detector. This technique has several advantages over the traditional methods, not the least of which is the absence of a large amount of foreign solvent introduced on the column. 11 refs., 7 figs.« less

Column chromatography isolation of nicotine from tobacco leaf extract (Nicotiana tabaccum L.)

NASA Astrophysics Data System (ADS)

Fathi, Raden Muhammad; Fauzantoro, Ahmad; Rahman, Siti Fauziyah; Gozan, Misri

2018-02-01

Restrictions on the use of dried tobacco leaf for cigarette production must be accompanied by the development of non-cigarette alternative products that are made from tobacco leaves. One of the alternative that can be done is to use the nicotine compound in tobacco leaf extract as medical product, such as Parkinson's medication or to be used as active substance in biopesticide. Nicotine was isolated using column chromatography method with the variation of mobile phase mixture ratio (petroleum ether and ethanol), started from 8:2, 6:4, 4:6, 2:8, to 0:10. All of the chromatographic fraction from each mobile phase's ratio was then tested qualitatively using thin layer chromatography (TLC) and also quantitatively using HPLC instrument. The column chromatography process could isolate 4.006% of nicotine compound from 4.19% tobacco leaf extract's nicotine. It is also known that ethanol is a good solution to be used as chromatography's mobile phase for nicotine isolation from tobacco leaf extract.

Method of using an electric field controlled emulsion phase contactor

DOEpatents

Scott, T.C.

1993-11-16

A system is described for contacting liquid phases comprising a column for transporting a liquid phase contacting system, the column having upper and lower regions. The upper region has a nozzle for introducing a dispersed phase and means for applying thereto a vertically oriented high intensity pulsed electric field. This electric field allows improved flow rates while shattering the dispersed phase into many micro-droplets upon exiting the nozzle to form a dispersion within a continuous phase. The lower region employs means for applying to the dispersed phase a horizontally oriented high intensity pulsed electric field so that the dispersed phase undergoes continuous coalescence and redispersion while being urged from side to side as it progresses through the system, increasing greatly the mass transfer opportunity. 5 figures.

Red Mexican grapefruit: a novel source for bioactive limonoids and their antioxidant activity.

PubMed

Mandadi, Kranthi K; Jayaprakasha, Guddadarangavvanahally K; Bhat, Narayan G; Patil, Bhimanagouda S

2007-01-01

Citrus limonoids have shown to inhibit the growth of cancer in colon, lung, mouth, stomach and breast in animal and cell culture studies. For the first time in the present study, an attempt has been made to isolate antioxidant fractions and five limonoids from red Mexican grapefruit seeds. Defatted seed powder was successively extracted with hexane, ethyl acetate (EtOAc), acetone, methanol (MeOH) and MeOH/water and the extracts were concentrated under vacuum. Radical scavenging activity of 1,1-diphenyl-2-picrylhydrazyl (DPPH) and total phenolic content were also measured for comparison with the antioxidant capacity in the phosphomolybdenum method for the above extracts. Acetone and MeOH extracts, respectively, showed the highest (85.7%) and lowest (53.3%) radical scavenging activity, at 500 ppm. The total phenolic contents were found to be highest in the acetone extract (15.94%) followed by the MeOH extract (5.92%), ethyl acetate extract (5.54%) and water extract (5.26%). Antioxidant capacity of the extracts as equivalents to ascorbic acid (micromol/g of the extract) was in the order, EtOAc extract > acetone extract > water extract > methanol extract. Furthermore, the EtOAC and acetone extracts were loaded onto silica gel columns to obtain four limonoid aglycons. MeOH fraction was loaded onto a dowex-50 and sepabeads resin column to obtain a limonoid glucoside. The purity of the isolated five compounds was analyzed by HPLC using a C18 column and UV detection at 210 nm. Finally, the structures of the compounds were identified as obacunone, nomilin, limonin, deacetylnomilin (DAN) and limonin-17-beta-D-glucopyranoside (LG) using 1H and 13C NMR studies.

Method for making a non-extractable stationary phase of polymer within a capillary column

DOEpatents

Springston, Stephen R.

1990-01-01

A method for coating interior capillary column surfaces, or packing material of a packed column, used for gas chromatography, with a stationary polymer phase that is cross-linked by exposing it to a low-temperature plasma that is uniformly distributed over the column or packing material for a predetermined period of time to effect the desired degree of cross-linking of the coating.

Low-density solvent based ultrasound-assisted emulsification microextraction and on-column derivatization combined with gas chromatography-mass spectrometry for the determination of carbamate pesticides in environmental water samples.

PubMed

Guo, Liang; Lee, Hian Kee

2012-04-27

A fast and efficient method for the determination of trace level of carbamate pesticides using a lower-density-than-water solvent for ultrasound-assisted emulsification microextraction coupled to on-column derivatization and analysis by GC-MS has been developed and studied. In this approach, a soft plastic Pasteur pipette was employed as a convenient extraction device. Fifty microliters of extraction solvent, of lower density than water, was injected into the sample solution held in the pipette. The latter was immediately immersed in an ultrasound water bath to form an emulsion. After 2 min extraction, the emulsion was fractionated into two layers by centrifugation. The upper layer (organic extract) could be collected conveniently by squeezing the bulb of the pipette, now held upside down, to move it into the narrow stem of the device, facilitating its retrieval for analysis. The extract was then combined with trimethylphenylammonium hydroxide and directly injected into a gas chromatography-mass spectrometry (GC-MS) system for on-column derivatization and analysis. The on-column derivatization provided an added convenience (since a separate step was not necessary). Parameters affecting the derivatization and extraction were investigated. Under the most favorable conditions, the method demonstrated high extraction efficiency with low limits of detection of between 0.01 and 0.1 μg/L, good linearity in the range of 0.05-50 μg/L, to 0.5-100 μg/L, and good repeatability (RSD below 9.2%, n=5). The proposed method was evaluated by determining carbamate pesticides in river water samples. Copyright © 2012 Elsevier B.V. All rights reserved.

Quantification of Complex Polycyclic Aromatic Hydrocarbon Mixtures in Standard Reference Materials Using GC×GC/ToF-MS

PubMed Central

Manzano, Carlos; Hoh, Eunha; Massey Simonich, Staci L.

2014-01-01

This research is the first to quantify complex PAH mixtures in NIST SRMs using comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC×GC/ToF-MS), with and without extract cleanup, and reports previously unidentified PAH isomers in the NIST SRMs. We tested a novel, high orthogonality GC column combination (LC-50×NSP-35), as well as with a commonly used column combination (Rtx-5ms×Rxi-17) for the quantification of a complex mixture of 85 different PAHs, including parent (PAHs), alkyl- (MPAHs), nitro- (NPAHs), oxy- (OPAHs), thio- (SPAHs), bromo- (BrPAHs), and chloro-PAHs (ClPAHs) in extracts from two standard reference materials: NIST SRM1650b (diesel particulate matter), with cleanup and NIST SRM1975 (diesel particulate extract), with and without extract cleanup. The LC-50×NSP-35 column combination resulted in an average absolute percent difference of 33.8%, 62.2% and 30.8% compared to the NIST certified PAH concentrations for NIST SRM1650b, NIST SRM1975 with cleanup and NIST SRM1975 without cleanup, while the Rtx-5ms×Rxi-17 resulted in an absolute percent difference of 38.6%, 67.2% and 79.6% for NIST SRM1650b, NIST SRM1975 with cleanup and NIST SRM1975 without cleanup, respectively. This GC×GC/ToF-MS method increases the number of PAHs detected and quantified in complex environmental extracts using a single chromatographic run. Without clean-up, 7 additional compounds were detected and quantified in NIST SRM1975 using the LC-50×NSP-35 column combination. These results suggest that the use of the LC-50×NSP-35 column combination in GC×GC/ToF-MS not only results in better chromatographic resolution and greater orthogonality for the separation of complex PAH mixtures, but can also be used for the accurate quantification of complex PAH mixtures in environmental extracts without cleanup. PMID:23932031

Modeling of rotating disc contactor (RDC) column

NASA Astrophysics Data System (ADS)

Ismail, Wan Nurul Aiffah; Zakaria, Siti Aisyah; Noor, Nor Fashihah Mohd; Sulong, Ibrahim; Arshad, Khairil Anuar

2014-12-01

Liquid-liquid extraction is one of the most important separation processes. Different kinds of liquid-liquid extractor such as Rotating Disc Contactor (RDC) Column being used in industries. The study of liquid-liquid extraction in an RDC column has become a very important subject to be discussed not just among chemical engineers but mathematician as well. In this research, the modeling of small diameter RDC column using the chemical system involving cumene/isobutryric asid/water are analyzed by the method of Artificial Neural Network (ANN). In the previous research, we begin the process of analyzed the data using methods of design of the experiments (DOE) to identify which factor and their interaction factor are significant and to determine the percentage of contribution of the variance for each factor. From the result obtained, we continue the research by discussed the development and validation of an artificial neural network model in estimating the concentration of continuous and concentration of dispersed outlet for an RDC column. It is expected that an efficient and reliable model will be formed to predict RDC column performance as an alternative to speed up the simulation process.

Analysis of trifluralin, methyl paraoxon, methyl parathion, fenvalerate and 2,4-D dimethylamine in pond water using solid-phase extraction

USGS Publications Warehouse

Swineford, D.M.; Belisle, A.A.

1989-01-01

A method was developed for the simultaneous extraction of trifluralin, methyl paraoxon, methyl parathion, fenvalerate, and 2,4-D dimethylamine salt in pond water using a solid-phase C18 column. After elution from the C18 column, the eluate was analyzed on a capillary gas chromatograph equipped with an electron-capture or flame photometric detector.

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of chlorinated pesticides in aquatic tissue by capillary-column gas chromatography with electron-capture detection

USGS Publications Warehouse

Leiker, Thomas J.; Madsen, J.E.; Deacon, J.R.; Foreman, W.T.

1995-01-01

A method for the determination of chlorinated organic compounds in aquatic tissue by dual capillary-column gas chromatography with electron-capture detection is described. Whole-body-fish or corbicula tissue is homogenized, Soxhlet extracted, lipid removed by gel permeation chromatography, and fractionated using alumina/silica adsorption chromatography. The extracts are analyzed by dissimilar capillary-column gas chromatography with electron-capture detection. The method reporting limits are 5 micrograms per kilogram (μg/kg) for chlorinated compounds, 50 μg/kg for polychlorinated biphenyls, and 200 μg/kg for toxaphene.

Solid-phase microextraction of phthalate esters in water sample using different activated carbon-polymer monoliths as adsorbents.

PubMed

Lirio, Stephen; Fu, Chung-Wei; Lin, Jhih-Yun; Hsu, Meng-Ju; Huang, Hsi-Ya

2016-07-13

In this study, the application of different activated carbon-polymer (AC-polymer) monoliths as adsorbents for the solid-phase microextraction (SPME) of phthalate esters (PAEs) in water sample were investigated. The activated carbon (AC) was embedded in organic polymers, poly(butyl methacrylate-co-ethylene dimethacrylate) (poly(BMA-EDMA)) or poly(styrene-co-divinylbenzene) (poly(STY-DVB)), via a 5-min microwave-assisted or a 15-min water bath heating polymerization. Preliminary investigation on the performance of the native poly(BMA-EDMA) and poly(STY-DVB) demonstrated remarkable adsorption efficiencies for PAEs. However, due to the strong hydrophobic, π-π, and hydrogen bonding interactions between the analytes and polymers, low extraction recoveries were achieved. In contrast, the presence of AC in native polymers not only enhanced the adsorption efficiencies but also assisted the PAE desorption, especially for AC-poly(STY-DVB) with extraction recovery ranged of 76.2-99.3%. Under the optimized conditions, the extraction recoveries for intra-, inter-day and column-to-column were in the range of 76.5-100.8% (<3.7% RSDs), 77.2-97.6% (<5.6% RSDs) and 75.5-99.7% (<6.2% RSDs), respectively. The developed AC-poly(STY-DVB) monolithic column showed good mechanical stability, which can be reused for more than 30 extraction times without any significant loss in the extraction recoveries of PAEs. The AC-poly(STY-DVB) monolithic column was successfully applied in SPME of PAEs in water sample with extraction recovery ranged of 78.8%-104.6% (<5.5% RSDs). Copyright © 2016 Elsevier B.V. All rights reserved.

Liquid chromatographic determination of the cyanobacterial toxin beta-n-methylamino-L-alanine in algae food supplements, freshwater fish, and bottled water.

PubMed

Scott, Peter M; Niedzwiadek, Barbara; Rawn, Dorothea F K; Lau, Ben P-Y

2009-08-01

Beta-N-Methylamino-L-alanine (BMAA) is a neurotoxin originally found in cycad seeds and now known to be produced by many species of freshwater and marine cyanobacteria. We developed a method for its determination in blue-green algae (BGA) food supplements, freshwater fish, and bottled water by using a strong cation-exchange, solid-phase extraction column for cleanup after 0.3 M trichloroacetic acid extraction of BGA supplements and fish. Bottled water was applied directly onto the solid-phase extraction column. For analysis of carbonated water, sonication and pH adjustment to 1.5 were needed. To determine protein-bound BMAA, the protein pellet left after extraction of the BGA supplement and fish was hydrolyzed by boiling with 6 M hydrochloric acid; BMAA was cleaned up on a C18 column and a strong cation-exchange, solid-phase extraction column. Determination of BMAA was by liquid chromatography of the fluorescent derivative formed with 9-fluorenylmethyl chloroformate. The method was validated by recovery experiments using spiking levels of 1.0 to 10 microg/g for BGA supplements, 0.5 to 5.0 microg/g for fish, and 0.002 microg/g for bottled water; mean recoveries were in the range of 67 to 89% for BGA supplements and fish, and 59 to 92% for bottled water. Recoveries of BMAA from spiked extracts of hydrolyzed protein from BGA supplements and fish ranged from 66 to 83%. The cleanup developed provides a useful method for surveying foods and supplements for BMAA and protein-bound BMAA.

Ionic liquid-based microwave-assisted extraction for the determination of flavonoid glycosides in pigeon pea leaves by high-performance liquid chromatography-diode array detector with pentafluorophenyl column.

PubMed

Wei, Wei; Fu, Yu-jie; Zu, Yuan-gang; Wang, Wei; Luo, Meng; Zhao, Chun-jian; Li, Chun-ying; Zhang, Lin; Wei, Zuo-fu

2012-11-01

In this study, an ionic liquid-based microwave-assisted extraction (ILMAE) followed by high-performance liquid chromatography-diode array detector with a pentafluorophenyl column for the extraction and quantification of eight flavonoid glycosides in pigeon pea leaves is described. Compared with conventional extraction methods, ILMAE is a more effective and environment friendly method for the extraction of nature compounds from herbal plants. Nine different types of ionic liquids with different cations and anions were investigated. The results suggested that varying the anion and cation had significant effects on the extraction of flavonoid glycosides, and 1.0 M 1-butyl-3-methylimidazolium bromide ([C4MIM]Br) solution was selected as solvent. In addition, the extraction procedures were also optimized using a series of single-factor experiments. The optimum parameters were obtained as follows: extraction temperature 60°C, liquid-solid ratio 20:1 mL/g and extraction time 13 min. Moreover, an HPLC method using pentafluorophenyl column was established and validated. Good linearity was observed with the regression coefficients (r(2)) more than 0.999. The limit of detection (LODs) (S/N = 3) and limit of quantification (LOQs) (S/N = 10) for the components were less than 0.41 and 1.47 μg/mL, respectively. The inter- and intraday precisions that were used to evaluate the reproducibility and relative standard deviation (RSD) values were less than 4.57%. The recoveries were between 97.26 and 102.69%. The method was successfully used for the analysis of samples of pigeon pea leaves. In conclusion, the developed ILMAE-HPLC-diode array detector using pentafluorophenyl column method can be applied for quality control of pigeon pea leaves and related medicinal products. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Fingerprinting of traditional Chinese medicines on the C18-Diol mixed-mode column in online or offline two-dimensional liquid chromatography on the single column modes.

PubMed

Wang, Qing; Tong, Ling; Yao, Lin; Zhang, Peng; Xu, Li

2016-06-05

In the present study, a mixed-mode stationary phase, C18-Diol, was applied for fingerprint analysis of traditional Chinese medicines. Hydrophobic, hydrogen bonding and electrostatic interactions were demonstrated to contribute the retention separately or jointly, which endowed the C18-Diol stationary phase with distinct selectivity compared to the bare C18 one. The separation of total alkaloids extracted from Fritillaria hupehensis was compared on the C18-Diol and conventional C18 column with the greater resolving power and better symmetry responses on the former one. Besides, a novel two-dimensional liquid chromatography on the single column (2D-LC-1C) was realized on C18-Diol with the offline mode for the alcohol extract of Fritillaria hupehensis and online mode for Ligusticum chuanxiong Hort. The early co-eluted extracted components with great polarity on the first dimension were reinjected on the same column and well separated on the second dimension. The results exhibited that the two complementary RPLC and HILIC modes on C18-Diol stationary phase enhanced the separation capacity and revealed more abundant chemical information of the sample, which was a powerful tool in analyzing complex herbal medicines. Copyright © 2016 Elsevier B.V. All rights reserved.

Determination of 3-hydroxypropylmercapturic acid in urine by three column-switching high-performance liquid chromatography with electrochemical detection using a diamond electrode.

PubMed

Higashi, Kyohei; Shibasaki, Mana; Kuni, Kyoshiro; Uemura, Takeshi; Waragai, Masaaki; Uemura, Kenichi; Igarashi, Kazuei; Toida, Toshihiko

2017-09-29

A three column-switching high-performance liquid chromatography (HPLC) using an electrochemical detector (ECD) equipped with a diamond electrode was established to determine 3-hydroxypropylmercapturic acid (3-HPMA) in urine. An extracted urine sample was consecutively fractionated using a strong anion-exchange column (first column) and a C8 column (second column) via a switching valve before application on an Octa Decyl Silyl (ODS) column (third column), followed by ECD analysis. The% recovery of 3-HPMA standard throughout the three-column process and limit of detection (LOD) were 94±1% and 0.1pmol, respectively. A solid phase extraction step is required for the sensitive analysis of 3-HPMA in urine by column-switching HPLC-ECD despite a decreased% recovery (55%) of urine sample spiked with 100pmol of 3-HPMA. To test the utility of our column-switching HPLC-ECD method, 3-HPMA levels of 27 urine samples were determined, and the correlation between HPLC-ECD and LC-Electrospray ionization (ESI)-MS/MS method was examined. As a result, the median values of μmol 3-HPMA/g Creatinine (Cre) in urine obtained by column-switching HPLC-ECD and LC-MS/MS were 2.19±2.12μmol/g Cre and 2.13±3.38μmol/g Cre, respectively, and the calibration curve (y=1.5171x-1.007) exhibited good linearity within a defined range (r 2 =0.907). These results indicate that the combination of column-switching HPLC and ECD is a powerful tool for the specific, reliable detection of 3-HPMA in urine. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of the cyanobacterial toxin cylindrospermopsin in algal food supplements.

PubMed

Liu, H; Scott, P M

2011-06-01

For the analysis of blue-green algal food supplements for cylindrospermopsin (CYN), a C18 solid-phase extraction column and a polygraphitized carbon solid-phase extraction column in series was an effective procedure for the clean-up of extracts. Determination of CYN was by liquid chromatography with ultraviolet light detection. At extract spiking levels of CYN equivalent to 25-500 µg g(-1), blue-green algal supplement recoveries were in the range 70-90%. CYN was not detected in ten samples of food supplements and one chocolate product, all containing blue-green algae. The limit of detection for the method was 16 µg g(-1), and the limit of quantification was 52 µg g(-1).

Extraction and speciation of arsenic in lacustrine sediments

USGS Publications Warehouse

Ficklin, W.H.

1990-01-01

Arsenic was partially extracted with 4.OM hydrochloric acid, from samples collected at 25-cm intervals in a 350-cm column of sediment at Milltown Reservoir, Montana and from a 60-cm core of sediment collected at the Cheyenne River Embayment of Lake Oahe, South Dakota. The sediment in both reservoirs is highly contaminated with arsenic. The extracted arsenic was separated into As(III) and As(V) on acetate form Dowex 1-X8 ion-exchange resin with 0.12M HCl eluent. Residual arsenic was sequentially extracted with KClO3 and HCl. Arsenic was determined by graphite-furnace atomic-absorption spectrometry. The analytical results define oxidized and reduced zones in the sediment columns. ?? 1990.

Method for making a non-extractable stationary phase of polymer within a capillary column

DOEpatents

Springston, S.R.

1990-10-30

A method is described for coating interior capillary column surfaces, or packing material of a packed column, used for gas chromatography, with a stationary polymer phase that is cross-linked by exposing it to a low-temperature plasma that is uniformly distributed over the column or packing material for a predetermined period of time to effect the desired degree of cross-linking of the coating. 7 figs.

Simple, specific analysis of organophosphorus and carbamate pesticides in sediments using column extraction and gas chromatography

USGS Publications Warehouse

Belisle, A.A.; Swineford, D.M.

1988-01-01

A simple, specific procedure was developed for the analysis of organophosphorus and carbamate pesticides in sediment. The wet soil was mixed with anhydrous sodium sulfate to bind water and the residues were column extracted in acetone:methylene chloride (1:l,v/v). Coextracted water was removed by additional sodium sulfate packed below the sample mixture. The eluate was concentrated and analyzed directly by capillary gas chromatography using phosphorus and nitrogen specific detectors. Recoveries averaged 93 % for sediments extracted shortly after spiking, but decreased significantly as the samples aged.

Effect of surfactant on single drop mass transfer for extraction of aromatics from lubricating oils

NASA Astrophysics Data System (ADS)

Izza, H.; Ben Abdessalam, S.; Korichi, M.

2018-03-01

Solvent extraction is an effective method for the reduction of the content of aromatic of lubricating oil. Frequently, with phenol, furfural, the NMP (out of N-methyl pyrrolidone). The power solvent and the selectivity can be still to increase while using surfactant as additive which facilitates the separation of phase and increases the yeild in raffinat. Liquid-liquid mass transfer coefficients for single freely rising drops in the presence of surfactant in an extraction column have been investigated. The surfactant used in this study was sodium lauryl ether sulfate (SLES). The experiments were performed by bubbling a solvent as a series of individual drops from the top of the column containing furfural-SLES solution. The column used in this experiment was made from glass with 17 mm inner diameter and a capacity of 125ml. The effects of the concentration of surfactant on the overall coefficient of mass transfer was investigated.

Isolation and identification of arctiin and arctigenin in leaves of burdock (Arctium lappa L.) by polyamide column chromatography in combination with HPLC-ESI/MS.

PubMed

Liu, Shiming; Chen, Kaoshan; Schliemann, Willibald; Strack, Dieter

2005-01-01

A simple method involving polyamide column chromatography in combination with HPLC-PAD and HPLC-ESI/MS for isolating and identifying two kinds of lignans, arctiin and arctigenin, in the leaves of burdock (Arctium lappa L.) has been established. After extraction of burdock leaves with 80% methanol, the aqueous phase of crude extracts was partitioned between water and chloroform and the aqueous phase was fractionated on a polyamide glass column. The fraction, eluting with 100% methanol, was concentrated and gave a white precipitate at 4 degrees C from which two main compounds were purified by semi-preparative HPLC. In comparison with the UV and ESI-MS spectra and the HPLC retention time of authentic standards, the compounds were determined to be arctiin and arctigenin. The extraction/separation technique was validated using an internal standard method.

Quasi-cw 20-W tunable 1-sec pulse CO/sub 2/ laser for optical pumping

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

Sharp, L.E.; Barkley, H.J.

1984-05-01

A four-section CO/sub 2/ laser is described which can produce 20 W in fundamental mode during a 1-sec pulse with a frequency tuning range of +- 300 MHz. It operates at 200-Torr pressure using sonic axial flow to inhibit the discharge column from filamenting. The input power density is 598 W cm/sup -3/ corresponding to an efficiency of 2%.

Dynamics of a Finite Liquid Oxygen (LOX) Column in a Pulsed Magnetic Field

NASA Technical Reports Server (NTRS)

Youngquist, Robert; Immer, Christopher; Lane, John; Simpson, James; Steinrock, T. (Technical Monitor)

2002-01-01

It is well known that liquid oxygen has a sufficient paramagnetic susceptibility that a strong magnetic field gradient can lift it in the earth's gravitational field. The movement of liquid oxygen is vital to the space program since it one of the primary oxidizers used for propulsion. Transport of liquid oxygen (LOX) via direct interaction of the magnetic fields (B field) with the fluid is a current topic of research and development at Kennedy Space Center, FL. This method of transporting (i.e. pumping) LOX may have particular advantages on Mars and other reduced gravitational environments, namely safety and reliability. This paper will address transport of a magnetic fluid, LOX, via phased-pulsed electromagnets acting on the edge of the column of fluid. The authors have developed a physical model from first-principles for the motion of a magnetic fluid in a particular U-tube geometry subjected to a pulsed magnetic field from an arbitrary solenoidal electromagnet. Experimental data that have been collected from the analogous geometry correlate well to that of the ab-initio calculations.

Evaluation of an airborne triple-pulsed 2 μm IPDA lidar for simultaneous and independent atmospheric water vapor and carbon dioxide measurements.

PubMed

Refaat, Tamer F; Singh, Upendra N; Yu, Jirong; Petros, Mulugeta; Ismail, Syed; Kavaya, Michael J; Davis, Kenneth J

2015-02-20

Water vapor and carbon dioxide are the most dominant greenhouse gases directly contributing to the Earth's radiation budget and global warming. A performance evaluation of an airborne triple-pulsed integrated path differential absorption (IPDA) lidar system for simultaneous and independent monitoring of atmospheric water vapor and carbon dioxide column amounts is presented. This system leverages a state-of-the-art Ho:Tm:YLF triple-pulse laser transmitter operating at 2.05 μm wavelength. The transmitter provides wavelength tuning and locking capabilities for each pulse. The IPDA lidar system leverages a low risk and technologically mature receiver system based on InGaAs pin detectors. Measurement methodology and wavelength setting are discussed. The IPDA lidar return signals and error budget are analyzed for airborne operation on-board the NASA B-200. Results indicate that the IPDA lidar system is capable of measuring water vapor and carbon dioxide differential optical depth with 0.5% and 0.2% accuracy, respectively, from an altitude of 8 km to the surface and with 10 s averaging. Provided availability of meteorological data, in terms of temperature, pressure, and relative humidity vertical profiles, the differential optical depth conversion into weighted-average column dry-air volume-mixing ratio is also presented.

Antimicrobial and cytotoxic constituents from leaves of Sapium baccatum.

PubMed

Ahmed, Yunus; Sohrab, Md Hossain; Al-Reza, Sharif M; Tareq, Faqir Shahidulla; Hasan, Choudhury M; Sattar, M A

2010-02-01

Six compounds, namely, Lupeol (1), Betulin (2), beta-Taraxerol (3), Taraxerone (4), Stigmasterol (5) and beta-Sitosterol (6) were isolated from the petroleum ether extract of the leaves of Sapium baccatum based on spectroscopic evidence. Lupeol (1), Betulin (2) and Stigmasterol (5) were isolated for the first time from this plant. The cytotoxic potential of the different solvent extracts (methanol, petroleum ether, carbon-tetrachloride and dichloromethane); six column fractions (F-4, F-7, F-10, F-12, F-18 and F-22) of petroleum ether extract and three pure compounds 1, 4 and 6 were determined by using brine shrimp lethality bioassay. The LC50 of all the tested samples were showed to be lethal to brine shrimp nauplii. However, petroleum ether, carbon-tetrachloride extract, column fractions F-4 and F-18 of petroleum ether extract and pure compound 6 showed quite potent activity in brine shrimp lethality bioassay with LC50 1.33, 1.35, 1.40, 1.58 and 1.58 microg/ml, respectively. These result suggested that they might be contain antitumor or pesticidal activity. Further, the methanol extract and four column fractions (F-7, F-12, F-18 and F-22) of petroleum ether showed significant activity against the tested microorganisms. Copyright 2009 Elsevier Ltd. All rights reserved.

Determination of Amino Acids in Cell Culture and Fermentation Broth Media Using Anion-Exchange Chromatography with Integrated Pulsed Amperometric Detection

PubMed Central

Hanko, Valoran P.; Heckenberg, Andrea; Rohrer, Jeffrey S.

2004-01-01

Anion-exchange chromatography with integrated pulsed amperometric detection (AE-IPAD) separates and directly detects amino acids, carbohydrates, alditols, and glycols in the same injection without pre- or post-column derivatization. These separations use a combination of NaOH and NaOH/sodium acetate eluents. We previously published the successful use of this technique, also known as AAA-Direct, to determine free amino acids in cell culture and fermentation broth media. We showed that retention of carbohydrates varies with eluent NaOH concentration differently than amino acids, and thus separations can be optimized by varying the initial NaOH concentration and its duration. Unfortunately, some amino acids eluting in the acetate gradient portion of the method were not completely resolved from system-related peaks and from unknown peaks in complex cell culture and fermentation media. In this article, we present changes in method that improve amino acid resolution and system ruggedness. The success of these changes and their compatibility with the separations previously designed for fermentation and cell culture are demonstrated with yeast extract-peptone-dextrose broth, M199, Dulbecco’s modified Eagle’s (with F-12), L-15 (Leibovitz), and McCoy’s 5A cell culture media. PMID:15585828

Recovery of 1,3-, 2,3-dichloropropenes, 1,2-dibromo-3-chloropropane, and o-, p-dichlorobenzenes from fatty and non-fat foodstuffs by liquid extraction technique.

PubMed

Daft, J L

1990-01-01

Food samples including fatty, non-fatty, grain-based, and nongrain-based types were fortified with the following five nematocides and fumigants: 1,3-dichloropropene, 2,3-dichloropropene, 1,2-dibromo-3-chloropropane, o-dichlorobenzene, and p-dichlorobenzene. Then, depending on sample consistency and type, the samples were diluted in, or extracted with organic solvent such as isooctane. A few of the high-fat extracts were passed through Florisil to remove excess fat or endogenous interferences. Analysis of the initial or cleaned up extracts was done by gas chromatography (GC) at 90 degrees C. The dichloropropenes were determined on 20% OV-101 columns with electron-capture and Hall electroconductivity detectors. The dichlorobenzenes and 1,2-dibromo-3-chloropropane, which elute beyond 30 min on the above columns, were determined on 5%-loaded columns using the same detectors. All five analytes were recovered from these techniques. Mean analyte recovery following a direct dilution or extraction was 83%, and following the Florisil cleanup step, was 52%. In 1986, a fumigant survey of about 200 foodstuffs by using this overall technique gave no findings of the five compounds studied here.

Determination of trigonelline, nicotinic acid, and caffeine in Yunnan Arabica coffee by microwave-assisted extraction and HPLC with two columns in series.

PubMed

Liu, Hongcheng; Shao, Jinliang; Li, Qiwan; Li, Yangang; Yan, Hong Mei; He, Lizhong

2012-01-01

A simple, rapid method was developed for simultaneous extraction of trigonelline, nicotinic acid, and caffeine from coffee, and separation by two chromatographic columns in series. The trigonelline, nicotinic acid, and caffeine were extracted with microwave-assisted extraction (MAE). The optimal conditions selected were 3 min, 200 psi, and 120 degrees C. The chromatographic separation was performed with two columns in series, polyaromatic hydrocarbon C18 (250 x 4.6 mm id, 5 microm particle size) and Bondapak NH2 (300 x 3.9 mm id, 5 microm particle size). Isocratic elution was with 0.02 M phosphoric acid-methanol (70 + 30, v/v) mobile phase at a flow rate of 0.8 mL/min. Good recoveries and RSD values were found for all analytes in the matrix. The LOD of the three compounds was 0.02 mg/L, and the LOQ was 0.005% in the matrix. The concentrations of trigonelline, nicotinic acid, and caffeine in instant coffee, roasted coffee, and raw coffee (Yunnan Arabica coffee) were assessed by MAE and hot water extraction; the correlation coefficients between concentrations of the three compounds obtained were close to 1.

Comparative study between extraction techniques and column separation for the quantification of sinigrin and total isothiocyanates in mustard seed.

PubMed

Cools, Katherine; Terry, Leon A

2012-07-15

Glucosinolates are β-thioglycosides which are found naturally in Cruciferae including the genus Brassica. When enzymatically hydrolysed, glucosinolates yield isothiocyanates and give a pungent taste. Both glucosinolates and isothiocyanates have been linked with anticancer activity as well as antifungal and antibacterial properties and therefore the quantification of these compounds is scientifically important. A wide range of literature exists on glucosinolates, however the extraction and quantification procedures differ greatly resulting in discrepancies between studies. The aim of this study was therefore to compare the most popular extraction procedures to identify the most efficacious method and whether each extraction can also be used for the quantification of total isothiocyanates. Four extraction techniques were compared for the quantification of sinigrin from mustard cv. Centennial (Brassica juncea L.) seed; boiling water, boiling 50% (v/v) aqueous acetonitrile, boiling 100% methanol and 70% (v/v) aqueous methanol at 70 °C. Prior to injection into the HPLC, the extractions which involved solvents (acetonitrile or methanol) were freeze-dried and resuspended in water. To identify whether the same extract could be used to measure total isothiocyanates, a dichloromethane extraction was carried out on the sinigrin extracts. For the quantification of sinigrin alone, boiling 50% (v/v) acetonitrile was found to be the most efficacious extraction solvent of the four tested yielding 15% more sinigrin than the water extraction. However, the removal of the acetonitrile by freeze-drying had a negative impact on the isothiocyanate content. Quantification of both sinigrin and total isothiocyanates was possible when the sinigrin was extracted using boiling water. Two columns were compared for the quantification of sinigrin revealing the Zorbax Eclipse to be the best column using this particular method. Copyright © 2012 Elsevier B.V. All rights reserved.

Comparison of extraction techniques of robenidine from poultry feed samples.

PubMed

Wilga, Joanna; Wasik, Agata Kot-; Namieśnik, Jacek

2007-10-31

In this paper, effectiveness of six different commonly applied extraction techniques for the determination of robenidine in poultry feed has been compared. The sample preparation techniques included shaking, Soxhlet, Soxtec, ultrasonically assisted extraction, microwave - assisted extraction and accelerated solvent extraction. Comparison of these techniques was done with respect to the recovery extraction, temperature and time, reproducibility and solvent consumption. Every single extract was subjected to clean - up using aluminium oxide column (Pasteur pipette filled with 1g of aluminium oxide), from which robenidine was eluted with 10ml of methanol. The eluate from the clean-up column was collected in a volumetric flask, and finally it was analysed by HPLC-DAD-MS. In general, all extraction techniques were capable of isolating of robenidine from poultry feed, but the recovery obtained using modern extraction techniques was higher than that obtained using conventional techniques. In particular, accelerated solvent extraction was more superior to other techniques, which highlights the advantages of this sample preparation technique. However, in routine analysis, shaking and ultrasonically assisted extraction is still the preferred method for the solution of robenidine and other coccidiostatics.

Nutrient and pollutant metals within earthworm residues are immobilized in soil during decomposition

PubMed Central

Richardson, J.B; Renock, D.J; Görres, J.H; Jackson, B.P; Webb, S.M; Friedland, A.J

2016-01-01

Earthworms are known to bioaccumulate metals, making them a potential vector for metal transport in soils. However, the fate of metals within soil upon death of earthworms has not been characterized. We compared the fate of nutrient (Ca, Mg, Mn) and potentially toxic (Cu, Zn, Pb) metals during decomposition of Amynthas agrestis and Lumbricus rubellus in soil columns. Cumulative leachate pools, exchangeable pools (0.1 M KCl + 0.01 M acetic acid extracted), and stable pools (16 M HNO3 + 12 M HCl extracted) were quantified in the soil columns after 7, 21, and 60 days of decomposition. Soil columns containing A. agrestis and L. rubellus had significantly higher cumulative leachate pools of Ca, Mn, Cu, and Pb than Control soil columns. Exchangeable and stable pools of Cu, Pb, and Zn were greater for A. agrestis and L. rubellus soil columns than Control soil columns. However, we estimated that > 98 % of metals from earthworm residues were immobilized in the soil in an exchangeable or stable form over the 60 days using a mass balance approach. Micro-XRF images of longitudinal thin sections of soil columns after 60 days containing A. agrestis confirm metals immobilization in earthworm residues. Our research demonstrates that nutrient and toxic metals are stabilized in soil within earthworm residues. PMID:28163331

Microwave assisted solvent extraction and coupled-column reversed-phase liquid chromatography with UV detection use of an analytical restricted-access-medium column for the efficient multi-residue analysis of acidic pesticides in soils.

PubMed

Hogendoom, E A; Huls, R; Dijkman, E; Hoogerbrugge, R

2001-12-14

A screening method has been developed for the determination of acidic pesticides in various types of soils. Methodology is based on the use of microwave assisted solvent extraction (MASE) for fast and efficient extraction of the analytes from the soils and coupled-column reversed-phase liquid chromatography (LC-LC) with UV detection at 228 nm for the instrumental analysis of uncleaned extracts. Four types of soils, including sand, clay and peat, with a range in organic matter content of 0.3-13% and ten acidic pesticides of different chemical families (bentazone, bromoxynil, metsulfuron-methyl, 2,4-D, MCPA, MCPP, 2,4-DP, 2,4,5-T, 2,4-DB and MCPB) were selected as matrices and analytes, respectively. The method developed included the selection of suitable MASE and LC-LC conditions. The latter consisted of the selection of a 5-microm GFF-II internal surface reversed-phase (ISRP, Pinkerton) analytical column (50 x 4.6 mm, I.D.) as the first column in the RAM-C18 configuration in combination with an optimised linear gradient elution including on-line cleanup of sample extracts and reconditioning of the columns. The method was validated with the analysis of freshly spiked samples and samples with aged residues (120 days). The four types of soils were spiked with the ten acidic pesticides at levels between 20 and 200 microg/kg. Weighted regression of the recovery data showed for most analyte-matrix combinations, including freshly spiked samples and aged residues, that the method provides overall recoveries between 60 and 90% with relative standard deviations of the intra-laboratory reproducibility's between 5 and 25%; LODs were obtained between 5 and 50 microg/kg. Evaluation of the data set with principal component analysis revealed that the parameters (i) increase of organic matter content of the soil samples and (ii) aged residues negatively effect the recovery of the analytes.

Efficient extraction and preparative separation of four main isoflavonoids from Dalbergia odorifera T. Chen leaves by deep eutectic solvents-based negative pressure cavitation extraction followed by macroporous resin column chromatography.

PubMed

Li, Lu; Liu, Ju-Zhao; Luo, Meng; Wang, Wei; Huang, Yu-Yan; Efferth, Thomas; Wang, Hui-Mei; Fu, Yu-Jie

2016-10-15

In this study, green and efficient deep eutectic solvent-based negative pressure cavitation-assisted extraction (DES-NPCE) followed by macroporous resin column chromatography was developed to extract and separate four main isoflavonoids, i.e. prunetin, tectorigenin, genistein and biochanin A from Dalbergia odorifera T. Chen leaves. The extraction procedure was optimized systematically by single-factor experiments and a Box-Behnken experimental design combined with response surface methodology. The maximum extraction yields of prunetin, tectorigenin, genistein and biochanin A reached 1.204, 1.057, 0.911 and 2.448mg/g dry weight, respectively. Moreover, the direct enrichment and separation of four isoflavonoids in DES extraction solution was successfully achieved by macroporous resin AB-8 with recovery yields of more than 80%. The present study provides a convenient and efficient method for the green extraction and preparative separation of active compounds from plants. Copyright © 2016 Elsevier B.V. All rights reserved.

Column carbon dioxide and water vapor measurements by an airborne triple-pulse integrated path differential absorption lidar: novel lidar technologies and techniques with path to space

NASA Astrophysics Data System (ADS)

Singh, U. N.; Petros, M.; Refaat, T. F.; Yu, J.; Ismail, S.

2017-09-01

The 2-micron wavelength region is suitable for atmospheric carbon dioxide (CO2) measurements due to the existence of distinct absorption features for the gas at this wavelength region [1]. For more than 20 years, researchers at NASA Langley Research Center (LaRC) have developed several high-energy and high repetition rate 2-micron pulsed lasers [2]. Currently, LaRC team is engaged in designing, developing and demonstrating a triple-pulsed 2-micron direct detection Integrated Path Differential Absorption (IPDA) lidar to measure the weighted-average column dry-air mixing ratios of carbon dioxide (XCO2) and water vapor (XH2O) from an airborne platform [1, 3-5]. This novel technique allows measurement of the two most dominant greenhouse gases, simultaneously and independently, using a single instrument. This paper will provide status and details of the development of this airborne 2-micron triple-pulse IPDA lidar. The presented work will focus on the advancement of critical IPDA lidar components. Updates on the state-of-the-art triple-pulse laser transmitter will be presented including the status of seed laser locking, wavelength control, receiver and detector upgrades, laser packaging and lidar integration. Future plans for IPDA lidar ground integration, testing and flight validation will also be discussed. This work enables new Earth observation measurements, while reducing risk, cost, size, volume, mass and development time of required instruments.

Space-Based CO2 Active Optical Remote Sensing using 2-μm Triple-Pulse IPDA Lidar

NASA Astrophysics Data System (ADS)

Singh, Upendra; Refaat, Tamer; Ismail, Syed; Petros, Mulugeta

2017-04-01

Sustained high-quality column CO2 measurements from space are required to improve estimates of regional and global scale sources and sinks to attribute them to specific biogeochemical processes for improving models of carbon-climate interactions and to reduce uncertainties in projecting future change. Several studies show that space-borne CO2 measurements offer many advantages particularly over high altitudes, tropics and southern oceans. Current satellite-based sensing provides rapid CO2 monitoring with global-scale coverage and high spatial resolution. However, these sensors are based on passive remote sensing, which involves limitations such as full seasonal and high latitude coverage, poor sensitivity to the lower atmosphere, retrieval complexities and radiation path length uncertainties. CO2 active optical remote sensing is an alternative technique that has the potential to overcome these limitations. The need for space-based CO2 active optical remote sensing using the Integrated Path Differential Absorption (IPDA) lidar has been advocated by the Advanced Space Carbon and Climate Observation of Planet Earth (A-Scope) and Active Sensing of CO2 Emission over Nights, Days, and Seasons (ASCENDS) studies in Europe and the USA. Space-based IPDA systems can provide sustained, high precision and low-bias column CO2 in presence of thin clouds and aerosols while covering critical regions such as high latitude ecosystems, tropical ecosystems, southern ocean, managed ecosystems, urban and industrial systems and coastal systems. At NASA Langley Research Center, technology developments are in progress to provide high pulse energy 2-μm IPDA that enables optimum, lower troposphere weighted column CO2 measurements from space. This system provides simultaneous ranging; information on aerosol and cloud distributions; measurements over region of broken clouds; and reduces influences of surface complexities. Through the continual support from NASA Earth Science Technology Office, current efforts are focused on developing an aircraft-based 2-μm triple-pulse IPDA lidar for independent and simultaneous monitoring of CO2 and water vapor (H2O). Triple-pulse IPDA design, development and integration is based on the knowledge gathered from the successful demonstration of the airborne CO2 2-μm double-pulse IPDA lidar. IPDA transmitter enhancements include generating high-energy (80 mJ) and high repetition rate (50Hz) three successive pulses using a single pump pulse. IPDA receiver enhancement include an advanced, low noise (1 fW/Hz1/2) MCT e-APD detection system for improved measurement sensitivity. In place of H2O sensing, the triple-pulse IPDA can be tuned to measure CO2 with two different weighting functions using two on-lines and a common off-line. Modeling of a space-based high-energy 2-µm triple-pulse IPDA lidar was conducted to demonstrate CO2 measurement capability and to evaluate random and systematic errors. Projected performance shows <0.12% random error and <0.07% residual systematic error. These translate to near-optimum 0.5 ppm precision and 0.3 ppm bias in low-tropospheric column CO2 mixing ratio measurements from space for 10 second signal averaging over Railroad Valley reference surface using US Standard atmospheric model. In addition, measurements can be optimized by tuning on-lines based upon ground target scenarios, environment and science objectives. With 10 MHz detection bandwidth, surface ranging with an uncertainty of <3 m can be achieved as demonstrated from earlier airborne flights.

Simultaneous determination of intracellular UDP-sugars in hyaluronic acid-producing Streptococcus zooepidemicus.

PubMed

Franke, Lukáš; Čožíková, Dagmar; Smirnou, Dzianis; Hermannová, Martina; Hanová, Tereza; Růžičková, Andrea; Velebný, Vladimír

2015-08-01

Two chromatographic methods for the quantitative analysis of uridine diphosphate (UDP) sugars involved in hyaluronan pathway of Streptococcus zooepidemicus (SEZ) were developed and compared. The sample preparation protocol using centrifugation and extraction in hot ethanol was employed prior to the analyses. Separation was achieved using an anion exchange Spherisorb SAX column or a Shodex QA-825 column connected with a photodiode array (PDA) detector. To increase the throughput of the chromatography method employing the Spherisorb SAX column, the solid phase extraction (SPE) procedure was introduced. Method validation results displayed that limits of detection (LODs) of UDP-glucose (UDP-Glc), UDP-N-acetylglucosamine (UDP-GlcNAc) and UDP-glucuronic acid (UDP-GlcA) calculated according to QC Expert software were in the low micromolar range and the coefficient of correlation (R(2)) was above 0.997. However, the analytical technique using the Spherisorb SAX column resulted in 80-90% recoveries and low LODs (≤6.19μM), the Shodex QA-825 column showed better long-term stability and reproducible chromatographic properties (RSD≤5.60%). The Shodex QA-825 column was successfully used to monitor UDP-sugar levels during the growth rate of SEZ cells. Copyright © 2015 Elsevier B.V. All rights reserved.

Simultaneous determination of quinolones in fish by liquid chromatography coupled with fluorescence detection: comparison of sub-2 microm particles and conventional C18 columns.

PubMed

Zhang, Hong; Chen, Si; Lu, Yanbin; Dai, Zhiyuan

2010-07-01

A simple and effective multi-residue analysis method is presented for the extraction and determination of eleven quinolones (pipemidic acid, enoxacin, norfloxacin, ciprofloxacin, lomefloxacin, enrofloxacin, gatifloxacin, difloxacin, oxolinic acid, nalidixic acid and flumequine) in fish tissues. In this study, multi-residue separations on four columns packed with 5 microm or sub-2 microm particles were simultaneously developed for the purpose of comparison. Various gradients were optimized and best resolutions were achieved on each column. A short and sub-2 microm particle-sized HPLC column was chosen for its advantages in analysis time and column performance. Additionally, considering the matrix effect of the complex crude fish tissue, an effective extraction protocol was also established for sample pre-treatment procedure. Good recoveries (71-98%) were obtained from samples fortified with a mix of eleven quinolones at three levels, with satisfactory relative standard deviations and limits of detection. As a result, the sub-2 microm HPLC column and proposed analytical procedures have been evaluated and applied to the analysis of different fish tissues. Detectable residues were observed in 8 of 30 samples, at concentrations ranging from 4.74 to 23.27 microg/kg.

Physical versus chemical effects on bacterial and bromide transport as determined from on site sediment column pulse experiments

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

Hall, James A.; Mailloux, Brian J.; Onstott, Tullis C.

2005-02-01

Twenty eight bacterial and Br transport experiments were performed in the field to determine the effects of physical and chemical heterogeneity of the aquifer sediment. The experiments were performed using groundwater from two field locations to examine the effects of groundwater chemistry on transport. Groundwater was extracted from multilevel samplers and pumped through 7 cm long columns of intact sediment or re-packed sieved and coated or uncoated sediment from the underlying aquifer. Two bacterial strains, Comamonas sp. DA001 and Paenibacillus polymyxa FER-02, were injected along with Br into the influent end of the columns to examine the effect of cellmore » morphology and surface properties on bacterial transport. The effect of column sediment grain size and mineral coatings coupled with groundwater geochemistry were also delineated. Significant irreversible attachment of DA001 was observed in the Fe oxyhydroxide coated columns, but only in the sub-oxic groundwater where the concentrations of dissolved organic carbon (DOC) were ca. 1 ppm. In the oxic groundwater where DOC was ca. 8 ppm, little attachment of DA001 to the Fe oxyhydroxide coated columns was observed. This indicates that DOC can significantly reduce bacterial attachment due electrostatic interactions. The larger and more negatively charged FER-02 displayed increasing attachment with decreasing grain size regardless of DOC concentration, and modeling of FER-02 attachment revealed that the presence of Fe and Al coatings on the sediment also promoted attachment. Finally, the presence of Al coatings and Al containing minerals appeared to significantly retard the Br tracer regardless of the concentration of DOC. These findings suggest that DOC in shallow oxic groundwater aquifers can significantly enhance the transport of bacteria by reducing attachment to Fe, Mn and Al oxyhydroxides. This effect is profound for weakly charged, hydrophilic bacteria and may contribute to differences in observations between laboratory experiments verses field-scale investigations particularly if the groundwater pH remains circum-neutral and Fe oxyhydroxide phases exist. These observations validate the novel approach taken in the experiments outlined here of performing laboratory-scale experiments on site to facilitate the use of fresh groundwater and thus be more representative of in situ groundwater conditions.« less

Comparison of a novel passive sampler to standard water-column sampling for organic contaminants associated with wastewater effluents entering a New Jersey stream

USGS Publications Warehouse

Alvarez, D.A.; Stackelberg, P.E.; Petty, J.D.; Huckins, J.N.; Furlong, E.T.; Zaugg, S.D.; Meyer, M.T.

2005-01-01

Four water samples collected using standard depth and width water-column sampling methodology were compared to an innovative passive, in situ, sampler (the polar organic chemical integrative sampler or POCIS) for the detection of 96 organic wastewater-related contaminants (OWCs) in a stream that receives agricultural, municipal, and industrial wastewaters. Thirty-two OWCs were identified in POCIS extracts whereas 9-24 were identified in individual water-column samples demonstrating the utility of POCIS for identifying contaminants whose occurrence are transient or whose concentrations are below routine analytical detection limits. Overall, 10 OWCs were identified exclusively in the POCIS extracts and only six solely identified in the water-column samples, however, repetitive water samples taken using the standard method during the POCIS deployment period required multiple trips to the sampling site and an increased number of samples to store, process, and analyze. Due to the greater number of OWCs detected in the POCIS extracts as compared to individual water-column samples, the ease of performing a single deployment as compared to collecting and processing multiple water samples, the greater mass of chemical residues sequestered, and the ability to detect chemicals which dissipate quickly, the passive sampling technique offers an efficient and effective alternative for detecting OWCs in our waterways for wastewater contaminants.

Regenerated silica gel as stationary phase on vacuum column chromatography to purify temulawak’s extracts

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

Cahyono, Bambang; Maduwu, Ratna Dewi; Widayat,

Commercial silica gel only used once by many researchers and affected high cost for purification process, also less support the green chemistry program. This research focused in regeneration silica gel that used purification of temulawak’s extracts (Curcuma xanthorrhiza Roxb) by vacuum column chromatography. Sample extracts (contains 10.1195±0.5971% of curcuminoids) was purified by vacuum column chromatography (pressure: 45 kPa, column: 100mm on length and 16mm on diameter). Ethanol 96% and acetone were compared as eluent. The amount of solvent and yield of curcuminoids used as indicator purification. The silica gel was regenerated with heating in 600°C for 8 hours The silica gelsmore » were analyzed by IR spectroscopy and X-ray diffraction. Furthermore, regenerated silica gel was used as the stationary phase in vacuum column chromatography under the same conditions with the previous purification. All the purification experiments were performed in three repetitions. Based on regression equation, y=0.132x+0.0011 (r{sup 2}=0.9997) the yield of curcuminoids on purified products using ethanol as the eluent was improved 4.26% (to 14.3724±0.5749%) and by acetone was improved 3,03% (to 13.1450 ±0.6318%). The IR spectrum of both silica gel showed the same vibration profile and also there were three crystallinity peaks missing on its X-ray diffraction. Regenerated silica gel has the same performance with new silica gel in purification of temulawak’s extract: by ethanol has increased 4.08% (14.1947±0.7415%) and 2.93% (13.0447±0.4822) by acetone. In addition, all purification products showed similar TLC profiles. Purification using regenerated silica gel as the adsorbent on vacuum column chromatography has exactly same potential with the new silica gel.« less

Simultaneous multi-mycotoxin determination in nutmeg by ultrasound-assisted solid-liquid extraction and immunoaffinity column clean-up coupled with liquid chromatography and on-line post-column photochemical derivatization-fluorescence detection.

PubMed

Kong, Wei-Jun; Liu, Shu-Yu; Qiu, Feng; Xiao, Xiao-He; Yang, Mei-Hua

2013-05-07

A simple and sensitive analytical method based on ultrasound-assisted solid-liquid extraction and immunoaffinity column clean-up coupled with high performance liquid chromatography and on-line post-column photochemical derivatization-fluorescence detection (USLE-IAC-HPLC-PCD-FLD) has been developed for simultaneous multi-mycotoxin determination of aflatoxins B1, B2, G1, G2 (AFB1, AFB2, AFG1, AFG2) and ochratoxin A (OTA) in 13 edible and medicinal nutmeg samples marketed in China. AFs and OTA were extracted from nutmeg samples by ultrasonication using a methanol : water (80 : 20, v/v) solution, followed by an IAC clean-up step. Different USL extraction conditions, pre-processing ways for nutmeg sample and clean-up columns for mycotoxins, as well as HPLC-PCD-FLD parameters (mobile phase, column temperature, elution procedure, excitation and emission wavelengths) were optimized. This method, which was appraised for analyzing nutmeg samples, showed satisfactory results with reference to limits of detection (LODs) (from 0.02 to 0.25 μg kg(-1)), limits of quantification (LOQs) (from 0.06 to 0.8 μg kg(-1)), linear ranges (up to 30 ng mL(-1) for AFB1, AFG1 and OTA and 9 ng mL(-1) for AFB2 and AFG2), intra- and inter-day variability (all <2%) and average recoveries (from 79.6 to 90.8% for AFs and from 93.6 to 97.3% for OTA, respectively). The results of the application of developed method in nutmeg samples have elucidated that four samples were detected with contamination of AFs and one with OTA. AFB1 was the most frequently found mycotoxin in 30.8% of nutmeg samples at contamination levels of 0.73-16.31 μg kg(-1). At least two different mycotoxins were co-occurred in three samples, and three AFs were simultaneously detected in one sample.

Preparative electrophoresis with on-column optical fiber monitoring and direct elution into a minimized volume.

PubMed

Jackson, George W; Willson, Richard

2005-11-01

A "column-format" preparative electrophoresis device which obviates the need for gel extraction or secondary electro-elution steps is described. Separated biomolecules are continuously detected and eluted directly into a minimal volume of free solution for subsequent use. An optical fiber allows the species of interest to be detected just prior to elution from the gel column, and a small collection volume is created by addition of an ion-exchange membrane near the end of the column.

[Research on chemical constituents from stem of Gymnema sylvestre].

PubMed

Zhen, Han-shen; Zhu, Xue-yan; Lu, Ru-mei; Liang, Jie; Qiu, Qin; Meng, Qi-miao

2008-08-01

To study on the chemical constituents from the stem of Gymnema sylvestre. The constituents were extracted by percolation with ethanol. Then the extract was separated by systemic solvent separation methods. The part of n-butanol extract was isolated and purified by macroporous adsorptive resins, silica gel column chromatography, sephadex gel column chromatography and recrystallization. The isolated compounds were identified by spectrum methods. Eight compounds were isolated and identified as fallows: Conduritol A(I), 1-Heptadecanol(II), Stigmasterol glucoside(III), 1-Quercitol(IV), 1-Octadecanol(V), Potassium nitrate(VI), Lupeol cinnamate(VII), Stigmasterol(VIII). Chemical compounds II, III, V, VII are firstly obtained from this plant.

Progress of the ELISE test facility: towards one hour pulses in hydrogen

NASA Astrophysics Data System (ADS)

Wünderlich, D.; Fantz, U.; Heinemann, B.; Kraus, W.; Riedl, R.; Wimmer, C.; the NNBI Team

2016-10-01

In order to fulfil the ITER requirements, the negative hydrogen ion source used for NBI has to deliver a high source performance, i.e. a high extracted negative ion current and simultaneously a low co-extracted electron current over a pulse length up to 1 h. Negative ions will be generated by the surface process in a low-temperature low-pressure hydrogen or deuterium plasma. Therefore, a certain amount of caesium has to be deposited on the plasma grid in order to obtain a low surface work function and consequently a high negative ion production yield. This caesium is re-distributed by the influence of the plasma, resulting in temporal instabilities of the extracted negative ion current and the co-extracted electrons over long pulses. This paper describes experiments performed in hydrogen operation at the half-ITER-size NNBI test facility ELISE in order to develop a caesium conditioning technique for more stable long pulses at an ITER relevant filling pressure of 0.3 Pa. A significant improvement of the long pulse stability is achieved. Together with different plasma diagnostics it is demonstrated that this improvement is correlated to the interplay of very small variations of parameters like the electrostatic potential and the particle densities close to the extraction system.

Increase in the neutron yield from a dense plasma-focus experiment performed with a conical tip placed in the centre of the anode end

NASA Astrophysics Data System (ADS)

Kubes, P.; Paduch, M.; Cikhardt, J.; Cikhardtova, B.; Klir, D.; Kravarik, J.; Rezac, K.; Zielinska, E.; Sadowski, M. J.; Szymaszek, A.; Tomaszewski, K.; Zaloga, D.

2017-09-01

The paper describes the evolution of self-organized structures inside a pinched plasma column during the phase of the effective production of fusion neutrons, as observed in the mega-ampere plasma focus experiment performed with a conical tip placed in the centre of the anode face. In a comparison with the plane anode face configuration, the described anode shape facilitated transformations in the pinch column during the neutron production and increased the neutron yield several times. Simultaneously, it decreased the minimal diameter and the length of the pinched column, and it depressed the first neutron pulse. It also induced shorter pulses of X-rays and neutrons, which enabled the determination of a temporal difference between the emission of electron and deuteron beams. The fast electrons were produced mainly during a disruption of the pinch constriction, while the fast deuterons - during the formation and explosion of plasmoids. The paper also presents the temporal evolution of a current distribution in the plasmoid during the neutron production, as well as the appearance and stable positions of current filaments traces upon the surface of the conical anode tip.

Development of an efficient fractionation method for the preparative separation of sesquiterpenoids from Tussilago farfara by counter-current chromatography.

PubMed

Song, Kwangho; Lee, Kyoung Jin; Kim, Yeong Shik

2017-03-17

A novel application of counter-current chromatography (CCC) to enrich plant extracts using direct and continuous injection (CCC-DCI) was developed to fractionate sesquiterpenoids from the buds of Tussilago farfara L. In this study, an n-hexane-acetonitrile-water (HAcW) solvent system was separately pumped into the CCC column, and an extraction solution (45% acetonitrile) was directly and continuously injected into the CCC column. Since the extraction solution was used as a mobile phase in this method, solvent consumption could be greatly reduced. To enrich the extraction solution (315.9g/5.4L), only 4.2L water, 4.6L acetonitrile, and 1.2L n-hexane were used, including the extraction step. Finally, 6.8g of a sesquiterpenoid-enriched (STE) fraction was obtained from the crude extract (315.9g) of Tussilago farfara (1kg) in a single CCC run with a separation time of 8.5h. The sample injection capacity of CCC-DCI was greater than 300g; this amount of sample could not be handled in conventional CCC or other fractionation methods with the same column volume. Moreover, three major sesquiterpenoids (1: tussilagone, 2: 14-acetoxy-7β-(3'-ethyl cis-crotonoyloxy)-1α-(2'-methylburyryloxy)-notonipetranone, and 3: 7β-(3'-ethyl cis-crotonoyloxy)-1α-(2'-methylburyryloxy)-3, 14-dehydro-Z-notonipetranone) were purified from the STE fraction by CCC, and their chemical structures were elucidated by 1 H NMR and 13 C NMR. A quantification study was conducted, and the contents of compounds 1-3 in the CCC-DCI fraction were higher than those of conventional multi-step fractionations performed in series: solvent partitioning and open column chromatography. Furthermore, the average CCC-DCI recoveries were 96.1% (1), 96.9% (2), and 94.6% (3), whereas the open column chromatography recoveries were 77.7% (1), 66.5% (2), and 58.4% (3). The developed method demonstrates that CCC is a useful technique for enriching target components from natural products. Copyright © 2017 Elsevier B.V. All rights reserved.

Separation of Ellagitannin-Rich Phenolics from U.S. Pecans and Chinese Hickory Nuts Using Fused-Core HPLC Columns and Their Characterization.

PubMed

Gong, Yi; Pegg, Ronald B

2017-07-19

U.S. pecans and Chinese hickory nuts possess a wide array of phenolic constituents with potential health benefits including phenolic acids and proanthocyanidins. Only limited information is available, however, on their compositions. The present study optimized the separation performance and characterized the low-molecular-weight phenolic fractions of these nuts with C18 and pentafluorophenyl (PFP) fused-core LC columns by employing a kinetic approach. Although both types of reversed-phase columns demonstrated similar performance in general, the PFP column furnished greater plate numbers and superior peak shapes for the low-molecular-weight fractions as well as overall separations of ellagic acid derivatives. The high-molecular-weight fraction of pecans, analyzed by a 3-μm HILIC column, possessed more proanthocyanidins than the Chinese hickory nuts with dimers and trimers (31.4 and 18.34 mg/g crude extract, respectively) being present at the greatest levels. Chinese hickory nuts had lower proanthocyanidin content but possessed tetramers and pentamers at 4.46 and 4.01 mg/g crude extract, respectively.

Analysis of perfluorinated carboxylic acids in soils II: optimization of chromatography and extraction.

PubMed

Washington, John W; Henderson, W Matthew; Ellington, J Jackson; Jenkins, Thomas M; Evans, John J

2008-02-15

With the objective of detecting and quantitating low concentrations of perfluorinated carboxylic acids (PFCAs), including perfluorooctanoic acid (PFOA), in soils, we compared the analytical suitability of liquid chromatography columns containing three different stationary phases, two different liquid chromatography-tandem mass spectrometry (LC/MS/MS) systems, and eight combinations of sample-extract pretreatments, extractions and cleanups on three test soils. For the columns and systems we tested, we achieved the greatest analytical sensitivity for PFCAs using a column with a C(18) stationary phase in a Waters LC/MS/MS. In this system we achieved an instrument detection limit for PFOA of 270 ag/microL, equating to about 14 fg of PFOA on-column. While an elementary acetonitrile/water extraction of soils recovers PFCAs effectively, natural soil organic matter also dissolved in the extracts commonly imparts significant noise that appears as broad, multi-nodal, asymmetric peaks that coelute with several PFCAs. The intensity and elution profile of this noise is highly variable among soils and it challenges detection of low concentrations of PFCAs by decreasing the signal-to-noise contrast. In an effort to decrease this background noise, we investigated several methods of pretreatment, extraction and cleanup, in a variety of combinations, that used alkaline and unbuffered water, acetonitrile, tetrabutylammonium hydrogen sulfate, methyl-tert-butyl ether, dispersed activated carbon and solid-phase extraction. For the combined objectives of complete recovery and minimization of background noise, we have chosen: (1) alkaline pretreatment; (2) extraction with acetonitrile/water; (3) evaporation to dryness; (4) reconstitution with tetrabutylammonium-hydrogen-sulfate ion-pairing solution; (5) ion-pair extraction to methyl-tert-butyl ether; (6) evaporation to dryness; (7) reconstitution with 60/40 acetonitrile/water (v/v); and (8) analysis by LC/MS/MS. Using this method, we detected in all three of our test soils, endogenous concentrations of all of our PFCA analytes, C(6) through C(10)-the lowest concentrations being roughly 30 pg/g of dry soil for perfluorinated hexanoic and decanoic acids in an agricultural soil.

Determination of available phosphorus in soils by using a new extraction procedure and a flow injection amperometric system.

PubMed

Jakmunee, Jaroon; Junsomboon, Jaroon

2009-09-15

A new extraction procedure based on an off-line extraction column was proposed for extracting of available phosphorus from soils. The column was fabricated from a plastic syringe fitted at the bottom with a cotton wool and a piece of filter paper to support a soil sample. An aliquot (50 mL) of extracting solution (0.05 M HCl+0.0125 M H(2)SO(4)) was used to extract the sample under gravity flow and the eluate was collected in a polyethylene bottle. The extract was then analyzed for phosphorus contents by a simple flow injection amperometric system, employing a set of three-way solenoid valves as an injection valve. The method is based on the electrochemical reduction of 12-molybdophosphate which is produced on-line by the reaction of orthophosphate with acidic molybdate and the electrical current produced was directly proportional to the concentration of phosphate in range of 0.1-10.0 mg L(-1) PO(4)-P, with a detection limit of 0.02 mg L(-1). Relative standard for 11 replicate injections of 5 mg L(-1) PO(4)-P was 0.5%. A sample through put of 35 h(-1) was achieved, with consumption of 14 mg KCl, 10mg ammonium molybdate and 0.05 mL H(2)SO(4) per analysis. The detection system does not suffer from the interferences that are encountered in the photometric method such as colored substances, colloids, metal ions, silicate and refractive index effect (Schlieren effect). The results obtained by the column extraction procedure were well correlated with those obtained by the steady-state extraction procedure, but showed slightly higher extraction efficiency.

[Multi-residue method for screening of pesticides in crops by liquid chromatography with tandem mass spectrometry].

PubMed

Tanizawa, Haruna; Shima, Mikie; Ikehara, Chieko; Kobata, Masakazu; Sato, Motoaki

2005-10-01

A simple and rapid method was developed for the screening of 82 pesticides/metabolites in a wide variety of crops, using solid-phase extraction and liquid chromatography with tandem mass spectrometry (LC/MS/MS). After extraction with methanol, the filtered extracts were made up to 100 mL and a 2 mL aliquot was subjected to solid-phase extraction. Co-extractives were removed with a C18 mini-column, while pesticides were retained on 3 kinds of mini-columns (HLB, SAX, activated carbon), and then eluted with acetonitrile. Analysis was performed by LC/MS/MS, and MS acquisition parameters were established in positive and negative ESI modes. The utility of the method was demonstrated by the analysis of 6 crops (carrot, cabbage, onion, spinach, lemon, brown rice) and one mixed vegetable juice. Of 82 compounds tested, 75 in carrot and 62 in lemon were obtained with recoveries ranging from 70-120%. For all samples tested, 75 compounds could be obtained with recoveries of over 50%, and the detection limits of most compounds were lower than 0.01 microg/g. This method provides acceptable performance for analysis of these 75 compounds. Further, by using aliquots of the extracts with small-scale mini-columns, purified samples could be obtained. This proposed method with small matrix effects, is effective and suitable for screening of multiple residual pesticides by using LC/MS/MS.

[Determination of azoxystrobin in tea by HPLC].

PubMed

Chonan, T

2001-08-01

A determination method has been developed for azoxystrobin in tea by HPLC. Azoxystrobin was extracted from a sample with acetone, and the extract was passed through an alumina column to remove tannin. The eluate was concentrated to ca. 25 mL and passed through a Sep-Pak Vac tC18 to remove pigments. The eluate was cleaned-up by using liquid-liquid partition, and Florisil and silica-gel columns. The HPLC analysis for azoxystrobin was carried out on a C18 column with acetonitrile-water (9:11) as the mobile phase, with ultraviolet detection at 260 nm. The recovery of azoxystrobin fortified at the level of 0.4 microgram/g was 90.2% and the limit of determination was 0.2 microgram/g.

Advances in Pulsed Lidar Measurements of CO2 Column Concentrations from Aircraft and for Space

NASA Astrophysics Data System (ADS)

Abshire, J. B.; Ramanathan, A. K.; Allan, G. R.; Hasselbrack, W. E.; Riris, H.; Numata, K.; Mao, J.; Sun, X.

2016-12-01

We have demonstrated an improved pulsed, multiple-wavelength integrated path differential absorption lidar for measuring the tropospheric CO2 concentrations. The lidar measures the range resolved shape of the 1572.33 nm CO2 absorption line to scattering surfaces, including the ground and the tops of clouds. Airborne measurements have used both 30 and 15 fixed wavelength samples distributed across the line. Analysis estimates the lidar range and pulse energies at each wavelength 10 times per second. The retrievals solve for the CO2 absorption line shape and the column average CO2 concentrations by using radiative transfer calculations, the aircraft altitude and range to the scattering surface, and the atmospheric conditions. We compare these to CO2 concentrations from in-situ sensors. In recent campaigns the lidar used a step-locked laser diode source, and a new HgCdTe APD detector in the receiver. During August and September 2014 the ASCENDS campaign flew over the California Central Valley, a coastal redwood forest, desert areas, and above growing crops in Iowa. Analyses show the retrievals of lidar range and CO2 column absorption, and mixing ratio worked well when measuring over variable topography and through thin clouds and aerosols. The retrievals clearly show the decrease in CO2 concentration over growing cropland. Airborne lidar measurements of horizontal gradients of CO2 concentrations across Nevada, Colorado and Nebraska showed good agreement with those from a model of CO2 flux and transport (PCTM). In several flights the agreement of the lidar with the column average concentration was < 1ppm, with standard deviation of 0.9 ppm. Two additional flights were made in February 2016 using a larger laser spot size and an optimized receiver. These improved the sensitivity x3, and the retrievals show 0.7 ppm precision over the desert in 1 second averaging time. A summary of these results will be presented, along with on-going developments for a space version.

Pulsed Airborne Lidar Measurements of C02 Column Absorption

NASA Technical Reports Server (NTRS)

Abshire, James B.; Riris, Haris; Allan, Graham R.; Weaver, Clark J.; Mao, Jianping; Sun, Xiaoli; Hasselbrack, William E.; Rodriquez, Michael; Browell, Edward V.

2011-01-01

We report on airborne lidar measurements of atmospheric CO2 column density for an approach being developed as a candidate for NASA's ASCENDS mission. It uses a pulsed dual-wavelength lidar measurement based on the integrated path differential absorption (IPDA) technique. We demonstrated the approach using the CO2 measurement from aircraft in July and August 2009 over four locations. The results show clear CO2 line shape and absorption signals, which follow the expected changes with aircraft altitude from 3 to 13 km. The 2009 measurements have been analyzed in detail and the results show approx.1 ppm random errors for 8-10 km altitudes and approx.30 sec averaging times. Airborne measurements were also made in 2010 with stronger signals and initial analysis shows approx. 0.3 ppm random errors for 80 sec averaging times for measurements at altitudes> 6 km.

Progress on development of an airborne two-micron IPDA lidar for water vapor and carbon dioxide column measurements

NASA Astrophysics Data System (ADS)

Singh, Upendra N.; Petros, Mulugeta; Refaat, Tamer F.; Yu, Jirong; Antill, Charles W.; Taylor, Bryant D.; Bowen, Stephen C.; Welters, Angela M.; Remus, Ruben G.; Wong, Teh-Hwa; Reithmaier, Karl; Lee, Jane; Ismail, Syed

2017-09-01

An airborne 2-μm triple-pulse integrated path differential absorption (IPDA) lidar is currently under development at NASA Langley Research Center (LaRC). This lidar targets both atmospheric carbon dioxide (CO2) and water vapor (H2O) column measurements, simultaneously. Advancements in the development of this IPDA lidar are presented in this paper. Updates on advanced two-micron triple-pulse high-energy laser transmitter will be given including packaging and lidar integration status. In addition, receiver development updates will also be presented. This includes a state-of-the-art detection system integrated at NASA Goddard Space Flight Center. This detection system is based on a newly developed HgCdTe (MCT) electron-initiated avalanche photodiode (e-APD) array. Future plan for IPDA lidar system for ground integration, testing and flight validation will be discussed.

Progress on Development of an Airborne Two-Micron IPDA Lidar for Water Vapor and Carbon Dioxide Column Measurements

NASA Technical Reports Server (NTRS)

Singh, Upendra N.; Petros, Mulugeta; Refaat, Tamer F.; Yu, Jirong; Antill, Charles W.; Taylor, Bryant D.; Bowen, Stephen C.; Welters, Angela M.; Remus, Ruben G.; Wong, Teh-Hwa;

Optimization of passively mode-locked quasi-continuously diode-pumped Nd:GdVO4 laser in bounce geometry

NASA Astrophysics Data System (ADS)

Frank, Milan; Jelínek, Michal; Kubeček, Václav

2015-01-01

In this paper the operation of pulsed diode-pumped Nd:GdVO4 laser oscillator in bounce geometry passively modelocked using semiconductor saturable absorber mirror (SAM), generating microjoule level picosecond pulses at wavelength of 1063 nm, is reported. Optimization of the output coupling for generation either Q-switched mode locked pulse trains or cavity dumped single pulses with maximum energy was performed, which resulted in extraction of single pulses as short as 10 ps and energy of 20 uJ. In comparison with the previous results obtained with this Nd:GdVO4 oscillator and saturable absorber in transmission mode, the achieved pulse duration is five times shorter. Using different absorbers and parameters of single pulse extraction enables generation of the pulses with duration up to 100 ps with the energy in the range from 10 to 20 μJ.

Effect of pore water velocities and solute input methods on chloride transport in the undisturbed soil columns of Loess Plateau

NASA Astrophysics Data System (ADS)

Zhou, BeiBei; Wang, QuanJiu

2017-09-01

Studies on solute transport under different pore water velocity and solute input methods in undisturbed soil could play instructive roles for crop production. Based on the experiments in the laboratory, the effect of solute input methods with small pulse input and large pulse input, as well as four pore water velocities, on chloride transport in the undisturbed soil columns obtained from the Loess Plateau under controlled condition was studied. Chloride breakthrough curves (BTCs) were generated using the miscible displacement method under water-saturated, steady flow conditions. Using the 0.15 mol L-1 CaCl2 solution as a tracer, a small pulse (0.1 pore volumes) was first induced, and then, after all the solution was wash off, a large pulse (0.5 pore volumes) was conducted. The convection-dispersion equation (CDE) and the two-region model (T-R) were used to describe the BTCs, and their prediction accuracies and fitted parameters were compared as well. All the BTCs obtained for the different input methods and the four pore water velocities were all smooth. However, the shapes of the BTCs varied greatly; small pulse inputs resulted in more rapid attainment of peak values that appeared earlier with increases in pore water velocity, whereas large pulse inputs resulted in an opposite trend. Both models could fit the experimental data well, but the prediction accuracy of the T-R was better. The values of the dispersivity, λ, calculated from the dispersion coefficient obtained from the CDE were about one order of magnitude larger than those calculated from the dispersion coefficient given by the T-R, but the calculated Peclet number, Pe, was lower. The mobile-immobile partition coefficient, β, decreased, while the mass exchange coefficient increased with increases in pore water velocity.

Comprehensive two-dimensional gas chromatography using partial modulation via a pulsed flow valve with a short modulation period.

PubMed

Freye, Chris E; Bahaghighat, H Daniel; Synovec, Robert E

2018-01-15

Partial modulation via a pulsed flow valve for comprehensive two-dimensional (2D) gas chromatography (GC × GC) is demonstrated, producing narrow peak widths, 2 W b , on the secondary separation dimension, 2 D, coupled with short modulation periods, P M , thus producing a high peak capacity on the 2 D dimension, 2 n c . The GC × GC modulator is a pulse flow valve that injects a pulse of carrier gas at the specified P M , at the connection between the primary, 1 D, column and the 2 D column. Using a commercially available pulse flow valve, this injection technique performs a combination of vacancy chromatography and frontal analysis, whereby each pulse disturbance in the analyte concentration profile as it exits the 1 D column results in data that is readily converted into a 2 D separation. A three-step process converts the raw data into a format analogous to a GC × GC separation, incorporating signal differentiation, baseline correction and conversion to a GC × GC chromatogram representation. A 115-component test mixture with a wide range of boiling points (36-372°C) of nine compound classes is demonstrated using modulation periods of P M = 50, 100, 250, and 500ms, respectively. For the test mixture with a P M of 250ms, peak shapes on 2 D are symmetric with apparent 2 W b ranging from 12 to 45ms producing a 2 n c of ~ 10. Based on the average peak width of 0.93s on the 1 D separation for a time window of 400s, the 1 D peak capacity is 1 n c ∼ 430. Thus, the ideal 2D peak capacity n c,2D is 4300 or a peak capacity production of 650 peaks/min using the P M of 250ms. Additionally, for a P M of 50, 100 and 500ms, the 2 n c are 4, 7, and 12, respectively. Retention times on 2 D, 2 t R , are reproducible having standard deviations less than 1ms. Finally, the processed data is shown to be quantitative, with an average RSD of 4.7% for test analytes. Copyright © 2017 Elsevier B.V. All rights reserved.

Chromatographic analysis of Polygalae Radix by online hyphenating pressurized liquid extraction

NASA Astrophysics Data System (ADS)

Song, Yuelin; Song, Qingqing; Li, Jun; Shi, Shepo; Guo, Liping; Zhao, Yunfang; Jiang, Yong; Tu, Pengfei

2016-06-01

Practicing “green analytical chemistry” is of great importance when profiling the chemical composition of complex matrices. Herein, a novel hybrid analytical platform was developed for direct chemical analysis of complex matrices by online hyphenating pressurized warm water extraction followed by turbulent flow chromatography coupled with high performance liquid chromatography-tandem mass spectrometry (PWWE-TFC-LC-MS/MS). Two parallel hollow guard columns acted as extraction vessels connected to a long narrow polyether ether ketone tube, while warm water served as extraction solvent and was delivered at a flow rate of 2.5 mL/min to generate considerable back pressure at either vessel. A column oven heated both the solvent and crude materials. A TFC column, which is advantageous for the comprehensive trapping of small molecular substances from fluids under turbulent flow conditions, was employed to transfer analytes from the PWWE module to LC-MS/MS. Two electronic valves alternated each vessel between extraction and elution phases. As a proof-of-concept, a famous herbal medicine for the treatment of neurodegenerative disorders, namely Polygalae Radix, was selected for the qualitative and quantitative analyses. The results suggest that the hybrid platform is advantageous in terms of decreasing time, material, and solvent consumption and in its automation, versatility, and environmental friendliness.

FLUID CONTACTOR APPARATUS

DOEpatents

Spence, R.; Streeton, R.J.W.

1956-04-17

The fluid contactor apparatus comprises a cylindrical column mounted co- axially and adapted to rotate within a cylindrical vessel, for the purpose of extracting a solute from am aqueous solution by means of an organic solvent. The column is particularly designed to control the vortex pattern so as to reduce the height of the vortices while, at the same time, the width of the annular radius in the radial direction between the vessel and column is less than half the radius of the column. A plurality of thin annular fins are spaced apart along the rotor approximately twice the radial dimension of the column such that two contrarotating substantially circular vortices are contained within each pair of fins as the column is rotated.

High sensitivity detection of bisphenol A using liposome chromatography.

PubMed

Liu, Xue-Ying; Nakamura, Chikashi; Tanimoto, Itsuro; Miyake, Shiro; Nakamura, Noriyuki; Hirano, Takashi; Miyake, Jun

2006-09-18

An antibody column in tandem with a fluorescent dye entrapped liposome column was developed for highly sensitive detection of an endocrine disruptor, bisphenol A (BPA). Anti-BPA antibody was immobilized in a protein G column with orientation control. A derivative of BPA was conjugated to phospholipase A2 (PLA2). BPA sample solutions mixed with the BPA-PLA2 conjugates were injected on to the anti-BPA antibody column and competitive binding occurred in the antibody column. The amount of the free conjugate was proportional to the concentration of the BPA sample. The eluted conjugates were injected on to the second column gel on which calcein-entrapped liposomes were immobilized and the PLA2-catalyzed hydrolysis of liposomal phospholipids causing fluorescent dye leakage as a signal amplification. In this system, the mixture of BPA and BPA-PLA2 conjugate were incubated for 60 min in the anti-BPA column, and then the collected solution was applied to the liposome column. The BPA detection range of 0.02-140 ng mL(-1) was wider than 0.03-6.6 ng mL(-1) obtained by the method of competitive ELISA using the same antibody. Moreover, this system could be adapted to an HPLC system resulting in almost the same detection limit in online detection. The method could be applied to environmental samples, river water and soil extracts. The BPA concentration of 0.1 ng mL(-1) and 10 ng g(-1) was detectable in water and soil extract, respectively.

A heat-pulse flowmeter for measuring minimal discharge rates in boreholes

USGS Publications Warehouse

Hess, A.E.

1982-01-01

The U.S. Geological Survey has tested a borehole-configured heat-pulse flowmeter which has good low-velocity flow-measuring sensitivity. The flowmeter was tested in the laboratory in 51-, 102-, and 152-millimeter-diameter columns using water velocities ranging from 0.35 to 250 millimeters per second. The heat-pulse flowmeter also was tested in a 15-meter-deep granite test pit with controlled water flow, and in a 58-meter-deep borehole in sedimentary materials. The flowmeter's capability to detect and measure naturally occurring, low-velocity, thermally induced convection currents in boreholes was demonstrated. Further improvements to the heat-pulse-flowmeter system are needed to increase its reliability and improve its response through four-conductor logging cable.

Fast Ion extraction from the MedEBIS

NASA Astrophysics Data System (ADS)

Höltermann, H.; Becker, R.; Kleinod, M.; Müller, I.

2004-01-01

Cancer therapy synchrotrons profit from single turn injection in terms of size, costs and easy operation. The MEdically Dedicated EBIS (MEDEBIS), built in Frankfurt, will deliver short (~1.5 µs) and intense (~1.3 mA) pulses of highly charged light ions (C, N, O) to meet the requirements for therapy facilities. The MEDEBIS operates with an electron beam of 400 mA at 5 keV and a ratio of beam to drift tube of 1/20. Drift tube potentials up to 1.6 kV are switched in some 100 ns to deliver a 1.5 µs ion pulse at an axial field gradient of 6.5 kV/m. On extraction, all potentials applied to the drift tubes are set to a given primary potential to define the extraction gradient. During extraction the drift tubes are not held at constant voltage to avoid spreading out of the pulse due to the restoration of the full space charge depression at locations where ions have already been extracted. To locally distribute the action of the applied potentials the drift tubes are fully interpenetrating each other with tapered fingers. Combining these features result in a potential wall, which follows the extracted ion pulse and produces a compressed short ion pulse for single turn injection. In the future similar constructions could be considered for the RHIS EBIS device or proposed for LHC to provide the advantage with respect to lowest emittance and highest luminosity to the accelerators at BNL and CERN.

Validation of a Microscale Extraction and High Throughput UHPLC-QTOF-MS Analysis Method for Huperzine A in Huperzia

PubMed Central

Cuthbertson, Daniel; Piljac-Žegarac, Jasenka; Lange, Bernd Markus

2011-01-01

Herein we report on an improved method for the microscale extraction of huperzine A (HupA), an acetylcholinesterase-inhibiting alkaloid, from as little as 3 mg of tissue homogenate from the clubmoss Huperzia squarrosa (G. Forst.) Trevis with 99.95 % recovery. We also validated a novel UHPLC-QTOF-MS method for the high-throughput analysis of H. squarrosa extracts in only 6 min, which, in combination with the very low limit of detection (20 pg on column) and the wide linear range for quantification (20 to 10,000 pg on column), allow for a highly efficient screening of extracts containing varying amounts of HupA. Utilization of this methodology has the potential to conserve valuable plant resources. PMID:22275140

Characterization of new types of stationary phases for fast and ultra-fast liquid chromatography by signal processing based on AutoCovariance Function: a case study of application to Passiflora incarnata L. extract separations.

PubMed

Pietrogrande, Maria Chiara; Dondi, Francesco; Ciogli, Alessia; Gasparrini, Francesco; Piccin, Antonella; Serafini, Mauro

2010-06-25

In this study, a comparative investigation was performed of HPLC Ascentis (2.7 microm particles) columns based on fused-core particle technology and Acquity (1.7 microm particles) columns requiring UPLC instruments, in comparison with Chromolith RP-18e columns. The study was carried out on mother and vegetal tinctures of Passiflora incarnata L. on one single or two coupled columns. The fundamental attributions of the chromatographic profiles are evaluated using a chemometric procedure, based on the AutoCovariance Function (ACVF). Different chromatographic systems are compared in terms of their separation parameters, i.e., number of total chemical components (m(tot)), separation efficiency (sigma), peak capacity (n(c)), overlap degree of peaks and peak purity. The obtained results show the improvements achieved by HPLC columns with narrow size particles in terms of total analysis time and chromatographic efficiency: comparable performance are achieved by Ascentis (2.7 microm particle) column and Acquity (1.7 microm particle) column requiring UPLC instruments. The ACVF plot is proposed as a simplified tool describing the chromatographic fingerprint to be used for evaluating and comparing chemical composition of plant extracts by using the parameters D% - relative abundance of the deterministic component - and c(EACF) - similarity index computed on ACVF. Copyright 2010 Elsevier B.V. All rights reserved.

Development of a screening method for the determination of forty-nine priority pollutants in soil

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

Kiang, P.H.T.

1985-01-01

An extraction procedure followed by capillary GC-MS analysis was used to determine soil pollutants. Dual pH solutions with methylene chloride were used as extraction solvent system. Both base/neutral and acidic fractions were analyzed on the same fused silica 30 meter SPB-1 (SE-30) column. A GC-FID with a 60 meter wide-bore SPB-1 glass capillary column was used for quantitative analysis due to its larger sample capacity and higher sensitivity. The precision and accuracy for 5.1 ppm (51 ..mu..g/10 g) concentration in zero soil was less than 25% RSD. A headspace technique was also developed for the determination of volatile compounds. Themore » same instrumental conditions and columns were used as in the extraction procedure. The precision and accuracy for 3 grams soil sample spiked with 5.1 ppm (52 ..mu..g/10 mL) pollutant mixture in a 20 mL vial was less than 3% RSD.« less

Analytical investigations of seismic responses for reinforced concrete bridge columns subjected to strong near-fault ground motion

NASA Astrophysics Data System (ADS)

Su, Chin-Kuo; Sung, Yu-Chi; Chang, Shuenn-Yih; Huang, Chao-Hsun

2007-09-01

Strong near-fault ground motion, usually caused by the fault-rupture and characterized by a pulse-like velocity-wave form, often causes dramatic instantaneous seismic energy (Jadhav and Jangid 2006). Some reinforced concrete (RC) bridge columns, even those built according to ductile design principles, were damaged in the 1999 Chi-Chi earthquake. Thus, it is very important to evaluate the seismic response of a RC bridge column to improve its seismic design and prevent future damage. Nonlinear time history analysis using step-by-step integration is capable of tracing the dynamic response of a structure during the entire vibration period and is able to accommodate the pulsing wave form. However, the accuracy of the numerical results is very sensitive to the modeling of the nonlinear load-deformation relationship of the structural member. FEMA 273 and ATC-40 provide the modeling parameters for structural nonlinear analyses of RC beams and RC columns. They use three parameters to define the plastic rotation angles and a residual strength ratio to describe the nonlinear load-deformation relationship of an RC member. Structural nonlinear analyses are performed based on these parameters. This method provides a convenient way to obtain the nonlinear seismic responses of RC structures. However, the accuracy of the numerical solutions might be further improved. For this purpose, results from a previous study on modeling of the static pushover analyses for RC bridge columns (Sung et al. 2005) is adopted for the nonlinear time history analysis presented herein to evaluate the structural responses excited by a near-fault ground motion. To ensure the reliability of this approach, the numerical results were compared to experimental results. The results confirm that the proposed approach is valid.

Structural Characterisation of Acetogenins from Annona muricata by Supercritical Fluid Chromatography Coupled to High-Resolution Tandem Mass Spectrometry.

PubMed

Laboureur, Laurent; Bonneau, Natacha; Champy, Pierre; Brunelle, Alain; Touboul, David

2017-11-01

Acetogenins are plant polyketides known to be cytotoxic and proposed as antitumor candidates. They are also suspected to be alimentary neurotoxins. Their occurrence as complex mixtures renders their dereplication and structural identification difficult using liquid chromatography coupled to tandem mass spectrometry and efforts are required to improve the methodology. To develop a supercritical fluid chromatography (SFC) high-resolution tandem mass spectrometry method, involving lithium post-column cationisation, for the structural characterisation of Annonaceous acetogenins in crude extracts. The seeds of Annona muricata L. were extracted with methanol. Supercritical fluid chromatography of the extract, using a 2-ethylpyridine stationary phase column, was monitored using a high-resolution quadrupole time-of-flight mass spectrometer. Lithium iodide was added post-column in the make-up solvent. For comparison, the same extract was analysed using high-pressure liquid chromatography coupled to the same mass spectrometer, with a column based on solid core particles. Sensitivity was similar for both HPLC and SFC approaches. Retention behaviour and fragmentation pathways of three different isomer groups are described. A previously unknown group of acetogenins was also evidenced for the first time. The use of SFC-MS/MS allows the reduction of the time of analysis, of environmental impact and an increase in the chromatographic resolution, compared to liquid chromatography. This new methodology enlightened a new group of acetogenins, isomers of montanacin-D. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

Molecularly imprinted coated graphene oxide solid-phase extraction monolithic capillary column for selective extraction and sensitive determination of phloxine B in coffee bean.

PubMed

Zhai, Haiyun; Su, Zihao; Chen, Zuanguang; Liu, Zhenping; Yuan, Kaisong; Huang, Lu

2015-03-20

A method was developed to sensitively determine phloxine B in coffee bean by molecularly imprinted polymers (MIPs) coated graphene oxide (GO) solid-phase extraction (GO-MISPE) coupled with high-performance liquid chromatography and laser-induced fluorescence detection (HPLC-LIF). The GO-MISPE capillary monolithic column was prepared by water-bath in situ polymerization, using GO as supporting material, phloxine B, methacrylic acid (MAA), and ethylene dimethacrylate (EDMA) as template, functional monomer, and cross-linker, respectively. The properties of the homemade GO-MISPE capillary monolithic column, including capacity and specificity, were investigated under optimized conditions. The GO-MIPs were characterized by scanning electron microscopy (SEM) and Fourier transform-infrared spectroscopy (FT-IR). The mean recoveries of phloxine B in coffee bean ranged from 89.5% to 91.4% and the intra-day and inter-day relative standard deviation (RSD) values all ranged from 3.6% to 4.7%. Good linearity was obtained over 0.001-2.0 μg mL(-1) (r=0.9995) with the detection limit (S/N=3) of 0.075 ng mL(-1). Under the selected conditions, enrichment factors of over 90-fold were obtained and extraction on the monolithic column effectively cleaned up the coffee bean matrix. The results demonstrated that the proposed GO-MISPE HPLC-LIF method can be applied to sensitively determine phloxine B in coffee bean. Copyright © 2015 Elsevier B.V. All rights reserved.

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.

Studies on the use of sepharose-N-(6-aminohexanoyl)-2-amino-2-deoxy-D-glucopyranose for the large-scale purification of hepatic glucokinase.

PubMed Central

Holroyde, M J; Chesher, J M; Trayer, I P; Walker, D G

1976-01-01

The synthesis of N-(6-aminohexanoyl)-2-amino-2-deoxy-D-glucose is described and it was shown to be a competitive inhibitor (Ki, 0.75 mM) with respect to glucose of rat hepatic glucokinase (EC 2.7.1.2). After attachment to CNBr-activated Sepharose 4B, this derivative was able to remove glucokinase quantitatively from crude liver extracts and release it when the columns were developed with glucose, glucosamine, N-acetyl-glucosamine or KC1. Repeated exposure of the columns to liver extracts led to rapid loss in their effectiveness as affinity matrices because proteins other than glucokinase are bound to the columns. The nature of such protein binding and methods for the rejuvenation of "used" columns are discussed along with the effect of the mode of preparation of the Sepharose-ligand conjugate and the concentration of bound ligand on the purification of glucokinase. Glucose 6-phosphate dehydrogenase is cited as an example of both non-specific protein binding to the affinity column and of the importance of the control of ligand concentration in removing such non-specifically bound proteins. Some guidelines emerged that should be generally applicable to other systems, particularly those which involve affinity chromatography of enzymes that are present in tissue extracts in very low amounts and possess only a relatively low association constant for the immobilized ligand. PMID:1275893

Optimization methods of pulse-to-pulse alignment using femtosecond pulse laser based on temporal coherence function for practical distance measurement

NASA Astrophysics Data System (ADS)

Liu, Yang; Yang, Linghui; Guo, Yin; Lin, Jiarui; Cui, Pengfei; Zhu, Jigui

2018-02-01

An interferometer technique based on temporal coherence function of femtosecond pulses is demonstrated for practical distance measurement. Here, the pulse-to-pulse alignment is analyzed for large delay distance measurement. Firstly, a temporal coherence function model between two femtosecond pulses is developed in the time domain for the dispersive unbalanced Michelson interferometer. Then, according to this model, the fringes analysis and the envelope extraction process are discussed. Meanwhile, optimization methods of pulse-to-pulse alignment for practical long distance measurement are presented. The order of the curve fitting and the selection of points for envelope extraction are analyzed. Furthermore, an averaging method based on the symmetry of the coherence function is demonstrated. Finally, the performance of the proposed methods is evaluated in the absolute distance measurement of 20 μ m with path length difference of 9 m. The improvement of standard deviation in experimental results shows that these approaches have the potential for practical distance measurement.

Tall fescue seed extraction and partial purification of ergot alkaloids

PubMed Central

Ji, Huihua; Fannin, F.; Klotz, J.; Bush, Lowell

2014-01-01

Many substances in the tall fescue/endophyte association (Schedonorus arundinaceus/Epichloë coenophiala) have biological activity. Of these compounds only the ergot alkaloids are known to have significant mammalian toxicity and the predominant ergot alkaloids are ergovaline and ergovalinine. Because synthetically produced ergovaline is difficult to obtain, we developed a seed extraction and partial purification protocol for ergovaline/ergovalinine that provided a biologically active product. Tall fescue seed was ground and packed into several different sized columns for liquid extraction. Smaller particle size and increased extraction time increased efficiency of extraction. Our largest column was a 114 × 52 × 61 cm (W × L × D) stainless steel tub. Approximately 150 kg of seed could be extracted in this tub. The extraction was done with 80% ethanol. When the solvent front migrated to bottom of the column, flow was stopped and seed was allowed to steep for at least 48 h. Light was excluded from the solvent from the beginning of this step to the end of the purification process. Following elution, ethanol was removed from the eluate by evaporation at room temperature and the resulting syrup was freeze-dried. About 80% recovery of alkaloids was achieved with 18-fold increase in concentration of ergovaline. Initial purification of the dried product was accomplished by extracting with hexane/water (6:1, v/v). The aqueous fraction was extracted with chloroform, the aqueous layer discarded, after which the chloroform was removed with a resulting 20-fold increase of ergovaline. About 65% of the ergovaline was recovered from the chloroform residue for an overall recovery of 50%. The resultant partially purified ergovaline had biological activities in in vivo and in vitro bovine bioassays that approximate that of synthetic ergovaline. PMID:25566528

Tall fescue seed extraction and partial purification of ergot alkaloids

NASA Astrophysics Data System (ADS)

Bush, Lowell

2014-12-01

Many substances in the tall fescue/endophyte association (Schedonorus arundinaceus/Epichloë coenophiala) have biological activity. Of these compounds only the ergot alkaloids are known to have significant mammalian toxicity and the predominant ergot alkaloids are ergovaline and ergovalinine. Because synthetically produced ergovaline is difficult to obtain, we developed a seed extraction and partial purification protocol for ergovaline/ergovalinine that provided a biologically active product. Tall fescue seed was ground and packed into several different sized columns for liquid extraction. Smaller particle size and increased extraction time increased efficiency of extraction. Our largest column was a 114 × 52 × 61 cm (W×L×D) stainless steel tub. Approximately 150 kg of seed could be extracted in this tub. The extraction was done with 80% ethanol. When the solvent front migrated to bottom of the column, flow was stopped and seed was allowed to steep for at least 48 h. Light was excluded from the solvent from the beginning of this step to the end of the purification process. Following elution, ethanol was removed from the eluate by evaporation at room temperature. Resulting syrup was freeze-dried. About 80% recovery of alkaloids was achieved with 18-fold increase in concentration of ergovaline. Initial purification of the dried product was accomplished by extracting with hexane/water (6:1, v/v) and the hexane fraction was discarded. The aqueous fraction was extracted with chloroform, the aqueous layer discarded, after which the chloroform was removed with a resulting 20-fold increase of ergovaline. About 65% of the ergovaline was recovered from the chloroform residue for an overall recovery of 50%. The resultant partially purified ergovaline had biological activities in in vivo and in vitro bovine bioassays that approximate that of synthetic ergovaline.

A core-shell column approach to a comprehensive high-performance liquid chromatography phenolic analysis of Vitis vinifera L. and interspecific hybrid grape juices, wines, and other matrices following either solid phase extraction or direct injection.

PubMed

Manns, David C; Mansfield, Anna Katharine

2012-08-17

Four high-throughput reverse-phase chromatographic protocols utilizing two different core-shell column chemistries have been developed to analyze the phenolic profiles of complex matrices, specifically targeting juices and wines produced from interspecific hybrid grape cultivars. Following pre-fractionation via solid-phase extraction or direct injection, individual protocols were designed to resolve, identify and quantify specific chemical classes of compounds including non-anthocyanin monomeric phenolics, condensed tannins following acid hydrolysis, and anthocyanins. Detection levels ranging from 1.2 ppb to 27.5 ppb, analyte %RSDs ranging from 0.04 to 0.38, and linear ranges of quantitation approaching five orders of magnitude were achieved using conventional HPLC instrumentation. Using C(18) column chemistry, the non-anthocyanin monomeric protocol effectively separated a set of 16 relevant phenolic compounds comprised flavan-3-ols, hydroxycinnamic acids, and flavonols in under 14 min. The same column was used to develop a 15-min protocol for hydrolyzed condensed tannin analysis. Two anthocyanin protocols are presented, one utilizing the same C(18) column, best suited for anthocyanidin and monoglucoside analysis, the other utilizing a pentafluorophenyl chemistry optimized to effectively separate complex mixtures of coexisting mono- and diglucoside anthocyanins. These protocols and column chemistries have been used initially to explore a wide variety of complex phenolic matrices, including red and white juices and wines produced from Vitis vinifera and interspecific hybrid grape cultivars, juices, teas, and plant extracts. Each protocol displayed robust matrix responses as written, yet are flexible enough to be easily modified to suit specifically tailored analytical requirements. Copyright © 2012 Elsevier B.V. All rights reserved.

Modeling the Pulse Signal by Wave-Shape Function and Analyzing by Synchrosqueezing Transform

PubMed Central

Wang, Chun-Li; Yang, Yueh-Lung; Wu, Wen-Hsiang; Tsai, Tung-Hu; Chang, Hen-Hong

2016-01-01

We apply the recently developed adaptive non-harmonic model based on the wave-shape function, as well as the time-frequency analysis tool called synchrosqueezing transform (SST) to model and analyze oscillatory physiological signals. To demonstrate how the model and algorithm work, we apply them to study the pulse wave signal. By extracting features called the spectral pulse signature, and based on functional regression, we characterize the hemodynamics from the radial pulse wave signals recorded by the sphygmomanometer. Analysis results suggest the potential of the proposed signal processing approach to extract health-related hemodynamics features. PMID:27304979

Modeling the Pulse Signal by Wave-Shape Function and Analyzing by Synchrosqueezing Transform.

PubMed

Wu, Hau-Tieng; Wu, Han-Kuei; Wang, Chun-Li; Yang, Yueh-Lung; Wu, Wen-Hsiang; Tsai, Tung-Hu; Chang, Hen-Hong

2016-01-01

We apply the recently developed adaptive non-harmonic model based on the wave-shape function, as well as the time-frequency analysis tool called synchrosqueezing transform (SST) to model and analyze oscillatory physiological signals. To demonstrate how the model and algorithm work, we apply them to study the pulse wave signal. By extracting features called the spectral pulse signature, and based on functional regression, we characterize the hemodynamics from the radial pulse wave signals recorded by the sphygmomanometer. Analysis results suggest the potential of the proposed signal processing approach to extract health-related hemodynamics features.

Methods of analysis by the U. S. Geological Survey National Water Quality Laboratory - determination of organonitrogen herbicides in water by solid-phase extraction and capillary-column gas chromatography/mass spectrometry with selected-ion monitoring

USGS Publications Warehouse

Sandstrom, Mark W.; Wydoski, Duane S.; Schroeder, Michael P.; Zamboni, Jana L.; Foreman, William T.

1992-01-01

A method for the isolation of organonitrogen herbicides from natural water samples using solid-phase extraction and analysis by capillary-column gas chromatography/mass spectrometry with selected-ion monitoring is described. Water samples are filtered to remove suspended particulate matter and then are pumped through disposable solid-phase extraction cartridges containing octadecyl-bonded porous silica to remove the herbicides. The cartridges are dried using carbon dioxide, and adsorbed herbicides are removed from the cartridges by elution with 1.8 milliliters of hexaneisopropanol (3:1). Extracts of the eluants are analyzed by capillary-column gas chromatography/mass spectrometry with selected-ion monitoring of at least three characteristic ions. The method detection limits are dependent on sample matrix and each particular herbicide. The method detection limits, based on a 100-milliliter sample size, range from 0.02 to 0.25 microgram per liter. Recoveries averaged 80 to 115 percent for the 23 herbicides and 2 metabolites in 1 reagent-water and 2 natural-water samples fortified at levels of 0.2 and 2.0 micrograms per liter.

Chromatographic Separation, and Characteristics of Nucleic Acids from HeLa Cells

PubMed Central

Philipson, Lennart

1961-01-01

The application of the phenol-duponol method to extraction of nucleic acids from HeLa cells is described. Chromatography of the phenol extract on an esterified bovine serum albumin column with a salt gradient of sodium chloride gives separation of soluble RNA, DNA, and two different high molecular RNA fractions. Ultracentrifugation of the DNA eluted from the column gives a sedimentation coefficient (s 20 o,w) of 38, which agrees with ultracentrifugation data on the phenol extract. The eluted RNA appears polydisperse at low ionic strength, but at high ionic strength and after alcohol precipitation two fractions with the sedimentation coefficients of 16 and 25 to 29, respectively, were obtained. PMID:13735276

Cold column trapping-cloud point extraction coupled to high performance liquid chromatography for preconcentration and determination of curcumin in human urine.

PubMed

Rahimi, Marzieh; Hashemi, Payman; Nazari, Fariba

2014-05-15

A cold column trapping-cloud point extraction (CCT-CPE) method coupled to high performance liquid chromatography (HPLC) was developed for preconcentration and determination of curcumin in human urine. A nonionic surfactant, Triton X-100, was used as the extraction medium. In the proposed method, a low surfactant concentration of 0.4% v/v and a short heating time of only 2min at 70°C were sufficient for quantitative extraction of the analyte. For the separation of the extraction phase, the resulted cloudy solution was passed through a packed trapping column that was cooled to 0 °C. The temperature of the CCT column was then increased to 25°C and the surfactant rich phase was desorbed with 400μL ethanol to be directly injected into HPLC for the analysis. The effects of different variables such as pH, surfactant concentration, cloud point temperature and time were investigated and optimum conditions were established by a central composite design (response surface) method. A limit of detection of 0.066mgL(-1) curcumin and a linear range of 0.22-100mgL(-1) with a determination coefficient of 0.9998 were obtained for the method. The average recovery and relative standard deviation for six replicated analysis were 101.0% and 2.77%, respectively. The CCT-CPE technique was faster than a conventional CPE method requiring a lower concentration of the surfactant and lower temperatures with no need for the centrifugation. The proposed method was successfully applied to the analysis of curcumin in human urine samples. Copyright © 2014 Elsevier B.V. All rights reserved.

Validated hydrophilic interaction LC-MS/MS method for simultaneous quantification of dacarbazine and 5-amino-4-imidazole-carboxamide in human plasma.

PubMed

Liu, Yanhong; Zhang, Weihua; Yang, Yuhui

2008-10-19

A hydrophilic interaction high performance liquid chromatography-tandem mass spectrometric method has been developed and validated for simultaneous quantification of dacarbazine (DTIC) and its terminal metabolite, 5-amino-4-imidazole-carboxamide (AIC) in human plasma. The plasma samples are first extracted by a C8+SCX mixed-mode 96-well plate to extend the extraction stability of DTIC and AIC. The extracted residues are further cleaned by a primary and secondary amine (PSA) adsorbent for minimization of matrix effect. Analyses are done on an Amide-80 HPLC column coupled to a tandem mass spectrometer fitted with an atmospheric pressure turbo ion spray ionization interface in the positive-ion mode. Both DTIC and AIC have reproducible retention times on the Amide-80 HPLC column. This type of column not only has an excellent column life (over 4000 injections), but also has zero carryover effect. The injection volume should be limited at 10 microL or less to avoid the peak splitting. The validated concentration ranges are from 0.5 to 500 ng/mL for DTIC and from 2.0 to 500 ng/mL for AIC. The validated method has been successfully applied to determine the pharmacokinetic profiles for human patients receiving DTIC infusions.

Comparison of Passive Samplers for Monitoring Dissolved Organic Contaminants in Water Column Deployments

EPA Science Inventory

Nonionic organic contaminants (NOCs) are difficult to measure in the water column due to their inherent chemical properties resulting in low water solubility and high particle activity. Traditional sampling methods require large quantities of water to be extracted and interferen...

Short communication: Development of a novel method for the extraction of norbixin from whey and its subsequent quantification via high performance liquid chromatography.

PubMed

Campbell, R E; Boogers, I A L A; Drake, M A

2014-03-01

Norbixin is the primary carotenoid in annatto coloring, which imparts the desired orange color in Cheddar cheese. However, a portion of the colorant remains in the cheese whey and is undesirable; therefore, a bleaching step is often applied. Restrictions exist for norbixin concentrations in products destined for infant formula. As such, evaluation of norbixin concentrations in whey and whey ingredients is desirable. Current extraction methods are laborious and require solvents that are banned in many countries. The objective of this study was to develop a fast and inexpensive norbixin extraction and quantitation technique using approved solvents with similar sensitivity to current established methods. Instead of solvent extraction and column purification, acetonitrile was added directly to fluid wheys, retentates, and rehydrated whey protein concentrates. An isocratic mobile phase [70% acetonitrile and 30% water with 0.1% (wt/vol) formic acid] was used and, to increase sensitivity, a large volume (50 μL) was injected onto the column. The column used was a C18 column with a particle size of 2.6 μm and column length of 10 cm. The column inner diameter was 4.6mm and the pore size was 100 Ǻ. All of the previously described conditions allowed the run time to be only 4 min. The sample was sent through a photodiode array detector and quantified at 482 nm. Norbixin was quantified using external standard curves. The developed method had a >90% norbixin recovery in both milk and whey (9.39 μg/L-2.35 mg/L). The limit of detection of norbixin in fluid whey was 2.7 μg/kg and the limit of quantitation was 3.5 μg/kg, both of which are significantly lower than in previously described methods. The extracts were stable over 30 min at 21°C and stable over 24h at 4°C. Repeatability and precision of the method had relative standard deviations of less than 13%. The developed method provides time and cost savings for evaluation of norbixin concentration in whey and whey products. Copyright © 2014 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

Preparation of highly pure zeaxanthin particles from sea water-cultivated microalgae using supercritical anti-solvent recrystallization.

PubMed

Chen, Chao-Rui; Hong, Siang-En; Wang, Yuan-Chuen; Hsu, Shih-Lan; Hsiang, Daina; Chang, Chieh-Ming J

2012-01-01

Xanthophylls, including zeaxanthin, are considered dietary supplements with a potentially positive impact on age-related macular degeneration. Using pilot-scale column fractionation coupled with supercritical anti-solvent (SAS) recrystallization, highly pure zeaxanthin particulates were prepared from ultrasonic extracts of the microalgae, Nannochloropsis oculata, grown in sea water. Column partition chromatography increased the concentration of zeaxanthin from 36.2 mg/g of the ultrasonic extracts to 425.6 mg/g of the collected column fractions. A response surface methodology was systematically designed for the SAS process by changing feed concentration, CO(2) flow rate and anti-solvent pressure. Zeaxanthin-rich particles with a purity of 84.2% and a recovery of 85.3% were produced using supercritical anti-solvent recrystallization from the column eluate at a feed concentration of 1.5 mg/mL, CO(2) flow rate of 48.6 g/min and pressure of 135 bar. Copyright © 2011 Elsevier Ltd. All rights reserved.

Manipulation of the micro and macro-structure of beams extracted from cyclotrons

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

Laxdal, R.E.

1995-09-01

It is standard practice in cyclotrons to alter the extracted micro-pulse width by using center-region slits and/or by chopping the beam before injection. The macro-structure can also be varied by means of pulsed or sinusoidal deflection devices before injection and/or after extraction. All above methods, however, involve cutting away the unwanted beam, thus reducing the time-averaged intensity. This paper will focus on some methods used to alter the time structure of extracted beams without significant beam loss. For example radial gradients in the accelerating fields from rf cavities can be utilized to compress, expand or even split longitudinally the circulatingmore » particle bunches. The macro-structure of the extracted beam can be altered by employing resonant extraction methods and replacing the static magnetic bump with either a pulsed or a sinusoidal transverse perturbation. The methods are most suitable for H cyclotrons but may also be considered in a limited scope for cyclotrons using direct extraction. Results of computer simulations and beam tests on the TRIUMF 500 MeV H{sup {minus}} cyclotron will be presented.« less

Achieving high peak capacity production for gas chromatography and comprehensive two-dimensional gas chromatography by minimizing off-column peak broadening.

PubMed

Wilson, Ryan B; Siegler, W Christopher; Hoggard, Jamin C; Fitz, Brian D; Nadeau, Jeremy S; Synovec, Robert E

2011-05-27

By taking into consideration band broadening theory and using those results to select experimental conditions, and also by reducing the injection pulse width, peak capacity production (i.e., peak capacity per separation time) is substantially improved for one dimensional (1D-GC) and comprehensive two dimensional (GC×GC) gas chromatography. A theoretical framework for determining the optimal linear gas velocity (the linear gas velocity producing the minimum H), from experimental parameters provides an in-depth understanding of the potential for GC separations in the absence of extra-column band broadening. The extra-column band broadening is referred to herein as off-column band broadening since it is additional band broadening not due to the on-column separation processes. The theory provides the basis to experimentally evaluate and improve temperature programmed 1D-GC separations, but in order to do so with a commercial 1D-GC instrument platform, off-column band broadening from injection and detection needed to be significantly reduced. Specifically for injection, a resistively heated transfer line is coupled to a high-speed diaphragm valve to provide a suitable injection pulse width (referred to herein as modified injection). Additionally, flame ionization detection (FID) was modified to provide a data collection rate of 5kHz. The use of long, relatively narrow open tubular capillary columns and a 40°C/min programming rate were explored for 1D-GC, specifically a 40m, 180μm i.d. capillary column operated at or above the optimal average linear gas velocity. Injection using standard auto-injection with a 1:400 split resulted in an average peak width of ∼1.5s, hence a peak capacity production of 40peaks/min. In contrast, use of modified injection produced ∼500ms peak widths for 1D-GC, i.e., a peak capacity production of 120peaks/min (a 3-fold improvement over standard auto-injection). Implementation of modified injection resulted in retention time, peak width, peak height, and peak area average RSD%'s of 0.006, 0.8, 3.4, and 4.0%, respectively. Modified injection onto the first column of a GC×GC coupled with another high-speed valve injection onto the second column produced an instrument with high peak capacity production (500-800peaks/min), ∼5-fold to 8-fold higher than typically reported for GC×GC. Copyright © 2011 Elsevier B.V. All rights reserved.

Oxygen octahedra picker: A software tool to extract quantitative information from STEM images.

PubMed

Wang, Yi; Salzberger, Ute; Sigle, Wilfried; Eren Suyolcu, Y; van Aken, Peter A

2016-09-01

In perovskite oxide based materials and hetero-structures there are often strong correlations between oxygen octahedral distortions and functionality. Thus, atomistic understanding of the octahedral distortion, which requires accurate measurements of atomic column positions, will greatly help to engineer their properties. Here, we report the development of a software tool to extract quantitative information of the lattice and of BO6 octahedral distortions from STEM images. Center-of-mass and 2D Gaussian fitting methods are implemented to locate positions of individual atom columns. The precision of atomic column distance measurements is evaluated on both simulated and experimental images. The application of the software tool is demonstrated using practical examples. Copyright © 2016 The Authors. Published by Elsevier B.V. All rights reserved.

Isolation and purification of total RNA from Streptococcus mutans in suspension cultures and biofilms.

PubMed

Cury, Jaime Aparecido; Seils, Jennifer; Koo, Hyun

2008-01-01

The presence of extracellular polysaccharides matrix makes extraction and purification of RNA from Streptococcus mutans within biofilms challenging. In this study, several approaches to purify RNA extracted from S. mutans in suspension cultures and biofilms were examined. The combination of sonication (3 pulses of 30 s at 7 W), suspension in NAES buffer (50 mM sodium acetate buffer, 10 mM EDTA and 1% SDS; pH 5.0) and homogenization-mechanical cells disruption in NAES- acid phenol:chloroform, yielded 9.04 mg (or 0.52 mg) of crude preparation of RNA per 100 mg of total cell (or biofilm) dry-weight. The crude RNA preparations were subjected to various DNAse I treatments. The combination of DNAse I in silica-gel based column followed by recombinant DNase I in solution provided the best genomic DNA removal, resulting in 4.35 mg (or 0.06 mg) of purified RNA per 100 mg of total cell (or biofilm) dry-weight. The cDNAs generated from the purified RNA sample were efficiently amplified using gtfB S. mutans-specific primers. The results showed a method that yields high-quality RNA from both planktonic cells and biofilms of S. mutans in sufficient quantity and quality for real-time RT-PCR analyses.

Homestead Valley, California, aftershocks (March 17-18, 1979) recorded on portable seismographs

USGS Publications Warehouse

Perry-Huston, Sue; Eberhart-Phillips, Donna

1994-01-01

A method for the determination of chlorinated organic compounds in aquatic tissue by dual capillary-column gas chromatography with electron- capture detection is described. Whole-body-fish or corbicula tissue is homogenized, Soxhlet extracted, lipid removed by gel permeation chromatography, and fractionated using alumina/silica adsorption chromatography. The extracts are analyzed by dissimilar capillary-column gas chromatography with electron-capture detection. The method reporting limits are 5 micrograms per kilogram (ug/kg) for chlorinated compounds, 50 ug/kg for polychlorinated biphenyls, and 200 ug/kg for toxaphene.

Rapid, direct extraction of DNA from soils for PCR analysis using polyvinylpolypyrrolidone spin columns.

PubMed

Berthelet, M; Whyte, L G; Greer, C W

1996-04-15

Polyvinylpolypyrrolidone spin columns were used to rapidly purify crude soil DNA extracts from humic materials for polymerase chain reaction (PCR) analysis. The PCR detection limit for the tfdC gene, encoding chlorocatechol dioxygenase from the 2,4-dichlorophenoxyacetic acid degradation pathway, was 10(1)-10(2) cells/g soil in inoculated soils. The procedure could be applied to the amplification of biodegradative genes from indigenous microbial populations from a wide variety of soil types, and the entire analysis could be performed within 8 h.

Water column particulate matter: A key contributor to phosphorus regeneration in a coastal eutrophic environment, the Chesapeake Bay: Particulate phosphorus in the Chesapeake Bay

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

Li, Jiying; Reardon, Patrick; McKinley, James P.

Particulate phosphorus (PP) in the water column is an essential component of phosphorus (P) cycling in aquatic ecosystems yet its composition and transformations remain largely uncharacterized. To understand the roles of suspended particulates on regeneration of inorganic P (Pi) into the water column as well as sequestration into more stable mineral precipitates, we studied seasonal variation in both organic and inorganic P speciation in suspended particles in three sites in the Chesapeake Bay using sequential P extraction, 1D (31P) and 2D (1H-31P) nuclear magnetic resonance (NMR) spectroscopies, and electron microprobe analyses (EMPA). Remineralization efficiency of particulate P average 8% andmore » 56% in shallow and deep sites respectively, suggesting the importance of PP remineralization is in resupplying water column Pi. Strong temporal and spatial variability of organic P composition, distributions, and remineralization efficiency were observed relating to water column parameters such as temperature and redox conditions: concentration of orthophosphate monoesters and diesters, and diester-to-monoester (D/M) ratios decreased with depth. Both esters and the D/M ratios were lower in the hypoxic July and September. In contrast, pyrophosphate and orthophosphate increased with depth, and polyphosphates was high in the anoxic water column. Sequential extraction and EMPA analyses of the suspended particles suggest presence of Ca-bound phosphate in the water column. We hypothesize authigenic precipitation of carbonate fluorapatite and/or its precursor mineral(s) in Pi rich water column, supported by our thermodynamic calculations. Our results, overall, reveal the important role suspended particles play in P remineralization and P sequestration in the Chesapeake Bay water column, provide important implications on P bioavailability and P sinks in similar eutrophic coastal environments.« less

Mobilization and Transport of Organic Compounds from Reservoir Rock and Caprock in Geological Carbon Sequestration Sites

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

Zhong, Lirong; Cantrell, Kirk J.; Mitroshkov, Alexandre V.

2014-05-06

Supercritical CO2 (scCO2) is an excellent solvent for organic compounds, including benzene, toluene, ethyl-benzene, and xylene (BTEX), phenols, and polycyclic aromatic hydrocarbons (PAHs). Monitoring results from geological carbon sequestration (GCS) field tests has shown that organic compounds are mobilized following CO2 injection. Such results have raised concerns regarding the potential for groundwater contamination by toxic organic compounds mobilized during GCS. Knowledge of the mobilization mechanism of organic compounds and their transport and fate in the subsurface is essential for assessing risks associated with GCS. Extraction tests using scCO2 and methylene chloride (CH2Cl2) were conducted to study the mobilization of volatilemore » organic compounds (VOCs, including BTEX), the PAH naphthalene, and n-alkanes (n-C20 – n-C30) by scCO2 from representative reservoir rock and caprock obtained from depleted oil reservoirs and coal from an enhanced coal-bed methane recovery site. More VOCs and naphthalene were extractable by scCO2 compared to the CH2Cl2 extractions, while scCO2 extractable alkane concentrations were much lower than concentrations extractable by CH2Cl2. In addition, dry scCO2 was found to extract more VOCs than water saturated scCO2, but water saturated scCO2 mobilized more naphthalene than dry scCO2. In sand column experiments, moisture content was found to have an important influence on the transport of the organic compounds. In dry sand columns the majority of the compounds were retained in the column except benzene and toluene. In wet sand columns the mobility of the BTEX was much higher than that of naphthalene. Based upon results determined for the reservoir rock, caprock, and coal samples studied here, the risk to aquifers from contamination by organic compounds appears to be relatively low; however, further work is necessary to fully evaluate risks from depleted oil reservoirs.« less

Extraction, Purification, and Spectroscopic Characterization of a Mixture of Capsaicinoids

ERIC Educational Resources Information Center

Wagner, Carl E.; Cahill, Thomas M.; Marshall, Pamela A.

2011-01-01

This laboratory experiment provides a safe and effective way to instruct undergraduate organic chemistry students about natural-product extraction, purification, and NMR spectroscopic characterization. On the first day, students extract dried habanero peppers with toluene, perform a pipet silica gel column to separate carotenoids from…

Rapid mixed mode solid phase extraction method for the determination of acrylamide in roasted coffee by HPLC-MS/MS.

PubMed

Bortolomeazzi, Renzo; Munari, Marina; Anese, Monica; Verardo, Giancarlo

2012-12-15

In this work, a rapid and reliable purification method based on a single mixed solid phase extraction (SPE) column, for the determination of acrylamide in roasted coffee by liquid chromatography-tandem mass spectrometry, was developed. Deuterium labelled d(3)-acrylamide was used as internal standard. Acrylamide was extracted by 10 mL of water and the extract purified by a single SPE column consisting of 0.5 g of an in-house prepared mixture of C18, strong cation (SCX) and anion exchange (SAX) sorbents in the ratio 2/1.5/1.5 (w/w/w). The amount of the three sorbents was optimised in order to eliminate the main interfering compounds present in coffee extracts, such as melanoidins, trigonelline, chlorogenic acids and caffeine. The SPE procedure was very simple and consisted of pushing 1 mL of an aqueous coffee extract through the SPE column followed by 1 mL of water which was collected for the analysis. The method was tested on six samples of roasted coffee of different composition and roasting level. The repeatability of the method, expressed as relative standard deviation (n=6), was lower than 5%. The recovery of acrylamide at three spiked levels ranged from 92% to 95%. The limits of detection (LOD) and quantitation (LOQ) were 5 and 16 μg kg(-1), respectively. Copyright © 2012 Elsevier Ltd. All rights reserved.

Evaluation of mobile phase characteristics on three zwitterionic columns in hydrophilic interaction liquid chromatography mode for liquid chromatography-high resolution mass spectrometry based untargeted metabolite profiling of Leishmania parasites.

PubMed

Zhang, Rong; Watson, David G; Wang, Lijie; Westrop, Gareth D; Coombs, Graham H; Zhang, Tong

2014-10-03

It has been reported that HILIC column chemistry has a great effect on the number of detected metabolites in LC-HRMS-based untargeted metabolite profiling studies. However, no systematic investigation has been carried out with regard to the optimisation of mobile phase characteristics. In this study using 223 metabolite standards, we explored the retention mechanisms on three zwitterionic columns with varied mobile phase composition, demonstrated the interference from poor chromatographic peak shapes on the output of data extraction, and assessed the quality of chromatographic signals and the separation of isomers under each LC condition. As expected, on the ZIC-cHILIC column the acidic metabolites showed improved chromatographic performance at low pH which can be attributed to the opposite arrangement of the permanently charged groups on this column in comparison with the ZIC-HILIC column. Using extracts from the protozoan parasite Leishmania, we compared the numbers of repeatedly detected LC-HRMS features under different LC conditions with putative identification of metabolites not amongst the standards being based on accurate mass (±3ppm). Besides column chemistry, the pH of the mobile phase plays a key role in not only determining the retention mechanisms of solutes but also the output of the LC-HRMS data processing. Fast evaporation of ammonium carbonate produced less ion suppression in ESI source and consequently improved the detectability of the metabolites in low abundance in comparison with other ammonium salts. Our results show that the combination of a ZIC-pHILIC column with an ammonium carbonate mobile phase, pH 9.2, at 20mM in the aqueous phase or 10mM in both aqueous and organic mobile phase components, provided the most suitable LC conditions for LC-HRMS-based untargeted metabolite profiling of Leishmania parasite extracts. The signal reliability of the mass spectrometer used in this study (Exactive Orbitrap) was also investigated. Copyright © 2014 Elsevier B.V. All rights reserved.

Application of a simple column-switching ion chromatography technique for removal of matrix interferences and sensitive fluorescence determination of acidic compounds (pharmaceutical drugs) in complex samples.

PubMed

Muhammad, Nadeem; Subhani, Qamar; Wang, Fenglian; Guo, Dandan; Zhao, Qiming; Wu, Shuchao; Zhu, Yan

2017-09-15

This work illustrates the introduction of a simple, rugged and flexible column-switching ion chromatography (IC) technique for an automated on-line QuEChERS extracted samples extracts washing followed by sensitive fluorescence (FLD) determination of five acidic pharmaceutical drugs namely; clofibric acid (CLO), ibuprofen (IBU), aspirin (ASP), naproxen (NAP) and flurobrofen (FLU) in three complex samples (spinach, apple and hospital sewage sludge). An old anion exchange column IonPac ® AS11-HC was utilized as a pre-treatment column for on-line washing of inorganic and organic interferences followed by isocratic separation of five acidic drugs with another anion exchange IonPac ® AS12A analytical column by exploiting the column-switching technique. This novel method exhibited good linearity with correlation coefficients (r 2 ) for all drugs were in the range 0.976-0.996. The limit of detection and quantification of all five acidic drugs were in the range 0.024μg/kg to 8.70μg/kg and 0.082μg/kg to 0.029mg/kg, respectively, and better recoveries in the range 81.17-112.5% with percentage relative standard deviations (RSDs) less than 17.8% were obtained. This on-line sample pre-treatment method showed minimum matrix effect in the range of 0.87-1.25 except for aspirin. This simple rugged and flexible column-switching system required only 28min for maximum elimination of matrices and interferences in three complex samples extracts, isocratic separation of five acidic drugs and for the continuous regeneration of pre-treatment column prior to every subsequent analysis. Finally, this simple automated IC system was appeared so rugged and flexible, which can eliminate and wash out most of interference, impurities and matrices in complex samples, simply by adjusting the NaOH and acetonitrile concentration in washing mobile phase with maximum recoveries of acidic analytes of interest. Copyright © 2017. Published by Elsevier B.V.

Extraction of quasi-straightforward-propagating photons from diffused light transmitting through a scattering medium by polarization modulation

NASA Astrophysics Data System (ADS)

Horinaka, Hiromichi; Hashimoto, Koji; Wada, Kenji; Cho, Yoshio; Osawa, Masahiko

1995-07-01

The utilization of light polarization is proposed to extract quasi-straightforward-propagating photons from diffused light transmitting through a scattering medium under continuously operating conditions. Removal of a floor level normally appearing on the dynamic range over which the extraction capability is maintained is demonstrated. By use of pulse-based observations this cw scheme of extraction of quasi-straightforward-propagating photons is directly shown to be equivalent to the use of a temporal gate in the pulse-based operation.

Chip-based molecularly imprinted monolithic capillary array columns coated GO/SiO2 for selective extraction and sensitive determination of rhodamine B in chili powder.

PubMed

Zhai, Haiyun; Huang, Lu; Chen, Zuanguang; Su, Zihao; Yuan, Kaisong; Liang, Guohuan; Pan, Yufang

2017-01-01

A novel solid-phase extraction chip embedded with array columns of molecularly imprinted polymer-coated silanized graphene oxide (GO/SiO2-MISPE) was established to detect trace rhodamine B (RB) in chili powder. GO/SiO2-MISPE monolithic columns for RB detection were prepared by optimizing the supporting substrate, template, and polymerizing monomer under mild water bath conditions. Adsorption capacity and specificity, which are critical properties for the application of the GO/SiO2-MISPE monolithic column, were investigated. GO/SiO2-MIP was examined by scanning electron microscopy (SEM) and Fourier transform-infrared spectroscopy. The recovery and the intraday and interday relative standard deviations for RB ranged from 83.7% to 88.4% and 2.5% to 4.0% and the enrichment factors were higher than 110-fold. The chip-based array columns effectively eliminated impurities in chili powder, indicating that the chip-based GO/SiO2-MISPE method was reliable for RB detection in food samples using high-performance liquid chromatography. Accordingly, this method has direct applications for monitoring potentially harmful dyes in processed food. Copyright © 2016 Elsevier Ltd. All rights reserved.

Featuring of transient tunneling current by voltage pulse and application to an electrochemical biosensor

NASA Astrophysics Data System (ADS)

Yun, Jun Yeon; Lee, Won Cheol; Choi, Seong Wook; Park, Young June

2018-03-01

We suggest a voltage pulse method for detecting the transient tunneling current component (faradaic current component) in a metal/redox-active monolayer/electrolyte system. After applying the pulse to the metal electrode, the capacitive current prevails; therefore, it is difficult to extract the tunneling current, which carries information on the biochemical reactions occurring between the biomarkers in the electrolyte and the self-assembled monolayer (SAM) as the probe peptide system. Instead of waiting until the capacitive current diminishes, and thereby, the tunneling current also decreases, we try to extract the tunneling current in an early stage of the pulse. The method is based on the observation that the capacitive current becomes symmetrized in the positive and negative pulses after introducing the SAM on the metal electrode. When the energy level of the redox molecule is higher than the Fermi level of the metal under zero-bias condition, the tunneling current in the negative pulse can be extracted by subtracting the capacitive current obtained from the positive pulse, where the tunneling current is neglected. The experiment conducted for detecting trypsin as a biomarker shows that the method enhances the sensitivity and the specific-to-nonspecific ratio of the sensor device in the case of the nonspecific protein-abundant electrolyte solution, as evinced by cyclic voltammetry measurements in comparison.

Pulsed 2-micron Laser Transmitter For Carbon Dioxide Sensing From Space

NASA Astrophysics Data System (ADS)

Singh, U. N.; Yu, J.; Bai, Y.; Petros, M.

2011-12-01

Carbon dioxide (CO2) has been recognized as one of the most important greenhouse gases. It is essential for the study of global warming to accurately measure the CO2 concentration in the atmosphere and continuously record its variation. Studies of the carbon cycle are limited by the tools available to precisely measure CO2 concentrations by remote sensing. Active sensing, using the Integrated Path Differential Absorption (IPDA) approach, permits measurements day and night, at all latitudes and seasons. The development of a high pulse energy 2-μm laser transmitter for high-precision CO2 measurements from space leverages years of NASA investment in solid-state laser technology. Under NASA Laser Risk Reduction Program, funded by Earth Science Technology Office, researchers at NASA Langley Research Center developed an injection seeded, high repetition rate, Q-switched Ho:YLF laser transmitter for CO2 Differential Absorption Lidar/IPDA (profile/column) measurements from ground and airborne platforms. This master-slave laser system has high optical-to-optical efficiency and seeding success rate. NASA LaRC's 2-micron pulsed laser transmitter possesses advantages over current passive and CW active sensors. First, the pulsed format provides a built-in means for determining range to the scattering target and effectively filtering out the scattering from thin clouds and aerosols, thus eliminating a source of measurement bias. Second, by concentrating the laser energy into a pulse, sufficient backscatter signal strength can be obtained from aerosol scattering rather than relying on a hard target at a known distance. Third, the absorption line at the 2.05 μm band is ideally suited for the CO2 concentration measurement. In particular, the weighting function of 2 μm is optimum for measurement in the lower troposphere where the sources and sinks of CO2 are located. The planned laser transmitter development will lead to a Tm:Fiber pumped Ho:YLF laser transmitter capable of delivering 65 mJ at 50 Hz at on-line wavelength and 50 mJ at 50 Hz at off-line wavelength. The planned laser technology development and performance capabilities are a major step forward in the laser transmitter requirements called out in recent comprehensive system studies, e.g., the European Space Agency (ESA) exploration mission studies, A-SCOPE, for future CO2 column density measurements from space. The planned laser technology development is relevant to NASA's earth science priorities, such as NASA ASCENDS mission for space-based CO2 column density measurements. This presentation will provide an overview of the current status of laser transmitter development and describe future technology development to meet the transmitter requirement for a space-based column averaged measurement of CO2 concentration.

Rapid determination of fumigant and industrial chemical residues in food.

PubMed

Daft, J L

1988-01-01

A gas chromatographic (GC) method is described for the determination of 22 fumigant and industrial chemical residues in a variety of foods. The fumigants and industrial chemicals determined are methyl bromide, methylene chloride, carbon disulfide, chloroform, 1,1-dichloroethane, ethylene dichloride, methyl chloroform, carbon tetrachloride, methylene bromide, propylene dichloride, 2,3-dichloropropene, trichloroethylene, 1,3-dichloropropylene, 1,1,2-trichloroethane, chloropicrin, ethylene dibromide, tetrachloroethylene, propylene dibromide, 1,1,2,2-tetrachloroethane, p-dichlorobenzene, o-dichlorobenzene, and 1,2-dibromo-3-chloropropane. Except for the latter three, the fumigants are determined at 90 degrees C on 3.6 m 20% loaded OV-101 columns with electron-capture and Hall-electroconductivity detectors. The other 3 compounds (o-dichlorobenzene, p-dichlorobenzene, and 1,2-dibromo-3-chloropropane), which elute beyond 30 min on the above columns, are determined at 90 degrees C on 1.8 m 5% loaded OV-101 columns with the same detectors. The ng/g-level fortifications have an overall mean analyte recovery of 70% and a coefficient of variation of 40%. The variety of foods examined includes both fatty and nonfatty food types (e.g., off-the-shelf cooked and uncooked grain-based items, dairy products, fresh and canned fruits and vegetables, and meats). Samples are extracted and cleaned up according to fat content and food type. Samples containing less than 71% fat are extracted by using an aqueous: nonaqueous shakeout (20% acetone solution under isooctane). Most extracts (isooctanes) are analyzed directly. Extracts from samples containing from 21 to 70% fat (e.g., ground beef, pecans, and corn chips) are cleaned up further on micro-Florisil columns to remove excess fat. A few other samples containing more than 71% fat or oil (e.g., butter, salad dressing, and vegetable oil) are diluted directly in isooctane and, depending on the degree of dilution, can be cleaned up further on micro-Florisil columns. Also, clear beverages (e.g., soda and tea) are extracted directly with isooctane. These extraction and cleanup techniques were tested on 231 different table-ready foods. Three-hundred incurred residues of 10 different fumigants were found in 138 items examined; 93 items had no detectable residues. The main advantage of the method is rapid semiquantitative determination of multiple fumigants from all food types.

A novel convenient process to obtain a raw decaffeinated tea polyphenol fraction using a lignocellulose column.

PubMed

Sakanaka, Senji

2003-05-07

Lignocellulose prepared from sawdust was investigated for its potential application in obtaining a raw decaffeinated tea polyphenol fraction from tea extract. Tea polyphenols having gallate residues, namely, (-)epigallocatechin gallate (EGCg) and (-)epicatechin gallate (ECg), were adsorbed on the lignocellulose column, while caffeine was passed through it. Adsorbed polyphenols were eluted with 60% ethanol, and the elute was found to consist mainly of EGCg and ECg. The caffeine/EGCg ratio was 0.696 before lignocellulose column treatment, but it became 0.004 after the column treatment. These results suggest that the lignocellulose column provides a useful and convenient process of purification of tea polyphenol fraction accompanied by decaffeination.

Comparison of Passive Samplers for Monitoring Dissolved Organic Contaminants in Water Column Deployments NAC/SETAC 2012

EPA Science Inventory

Nonionic organic contaminants (NOCs) are difficult to measure in the water column due to their inherent chemical properties resulting in low water solubility and high particle activity. Traditional sampling methods require large quantities of water to be extracted and interferen...

Comparison of Passive Samplers for Monitoring Dissolved Organic Contaminants in Water Column Deployments (SETAC Europe 22nd Annual Meeting)

EPA Science Inventory

Nonionic organic contaminants (NOCs) are difficult to measure in the water column due to their inherent chemical properties resulting in low water solubility and high particle activity. Traditional sampling methods require large quantities of water to be extracted and interferen...

Protocol for Initial Purification of Bacteriocin

DTIC Science & Technology

2015-10-01

lysate/extract preparation, column purification, and a desalting . The peptide was tracked throughout the process using a soft agar overlay activity...tris PAGE. It is necessary to desalt those samples for 150-mM and 1-M fractions, by using dialysis or G10 sephadex columns, in order to prevent

Phenolic composition of pomegranate peel extracts using an LC-MS approach with silica hydride columns

USDA-ARS?s Scientific Manuscript database

The peels of different pomegranate cultivars (Molla Nepes, Parfianka, Purple Heart, Wonderful and Vkunsyi) were compared in terms of phenolic composition and total phenolics. Analyses were performed on two silica hydride-based stationary phases: phenyl and undecenoic acid columns. Quantitation was ...

Feasibility study of a space-based high pulse energy 2  μm CO2 IPDA lidar.

PubMed

Singh, Upendra N; Refaat, Tamer F; Ismail, Syed; Davis, Kenneth J; Kawa, Stephan R; Menzies, Robert T; Petros, Mulugeta

2017-08-10

Sustained high-quality column carbon dioxide (CO 2 ) atmospheric measurements from space are required to improve estimates of regional and continental-scale sources and sinks of CO 2 . Modeling of a space-based 2 μm, high pulse energy, triple-pulse, direct detection integrated path differential absorption (IPDA) lidar was conducted to demonstrate CO 2 measurement capability and to evaluate random and systematic errors. Parameters based on recent technology developments in the 2 μm laser and state-of-the-art HgCdTe (MCT) electron-initiated avalanche photodiode (e-APD) detection system were incorporated in this model. Strong absorption features of CO 2 in the 2 μm region, which allows optimum lower tropospheric and near surface measurements, were used to project simultaneous measurements using two independent altitude-dependent weighting functions with the triple-pulse IPDA. Analysis of measurements over a variety of atmospheric and aerosol models using a variety of Earth's surface target and aerosol loading conditions were conducted. Water vapor (H 2 O) influences on CO 2 measurements were assessed, including molecular interference, dry-air estimate, and line broadening. Projected performance shows a <0.35  ppm precision and a <0.3  ppm bias in low-tropospheric weighted measurements related to column CO 2 optical depth for the space-based IPDA using 10 s signal averaging over the Railroad Valley (RRV) reference surface under clear and thin cloud conditions.

Determination of strontium-90 in milk samples using a controlled precipitation clean-up step prior to ion-chromatography.

PubMed

Cobb, J; Warwick, P; Carpenter, R C; Morrison, R T

1995-12-01

Strontium-90 may be determined by beta-counting its yttrium-90 daughter following separation by ion-chromatography, using a three column system comprising a chelating concentrator column, a cation-exchange column and an anion-exchange separator column. The column system has previously been applied to the determination of strontium-90 in water and urine samples. The applicability of the system to the analysis of milk is hampered by the large concentrations of calcium present, which significantly reduces the extraction of yttrium-90 by the concentrator column. A maximum of approximately 200 mg of calcium can be present for the successful extraction of yttrium-90, which greatly limits the quantity of milk that can be analysed. The quantity of milk analysed can be increased by the inclusion of a controlled precipitation step prior to the ion-chromatographic separation. The precipitation is carried out on acid digested milk samples by the addition of ammonia solution until the addition of one drop causes a reduction in pH resulting in the precipitation of calcium hydrogenphosphate. Under these conditions, approximately 20% of the calcium present in the original milk sample is precipitated, yttrium-90 is precipitated whereas strontium-90 is not precipitated. Dissolution of the precipitate, followed by separation of yttrium-90 using the ion-chromatography system facilitates the analysis of a litre of milk with recoveries of greater than 80%.

Phenolic composition of pomegranate peel extracts using an liquid chromatography-mass spectrometry approach with silica hydride columns.

PubMed

Young, Joshua E; Pan, Zhongli; Teh, Hui Ean; Menon, Veena; Modereger, Brent; Pesek, Joseph J; Matyska, Maria T; Dao, Lan; Takeoka, Gary

2017-04-01

The peels of different pomegranate cultivars (Molla Nepes, Parfianka, Purple Heart, Wonderful and Vkunsyi) were compared in terms of phenolic composition and total phenolics. Analyses were performed on two silica hydride based stationary phases: phenyl and undecanoic acid columns. Quantitation was accomplished by developing a liquid chromatography with mass spectrometry approach for separating different phenolic analytes, initially in the form of reference standards and then with pomegranate extracts. The high-performance liquid chromatography columns used in the separations had the ability to retain a wide polarity range of phenolic analytes, as well as offering beneficial secondary selectivity mechanisms for resolving the isobaric compounds, catechin and epicatechin. The Vkunsyi peel extract had the highest concentration of phenolics (as determined by liquid chromatography with mass spectrometry) and was the only cultivar to contain the important compound punicalagin. The liquid chromatography with mass spectrometry data were compared to the standard total phenolics content as determined by using the Folin-Ciocalteu assay. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Multiclonal plastic antibodies for selective aflatoxin extraction from food samples.

PubMed

Bayram, Engin; Yılmaz, Erkut; Uzun, Lokman; Say, Rıdvan; Denizli, Adil

2017-04-15

Herein, we focused on developing a new generation of monolithic columns for extracting aflatoxin from real food samples by combining the superior features of molecularly imprinted polymers and cryogels. To accomplish this, we designed multiclonal plastic antibodies through simultaneous imprinting of aflatoxin subtypes B1, B2, G1, and G2. We applied Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), and spectrofluorimetry to characterize the materials, and conducted selectivity studies using ochratoxin A and aflatoxin M1 (a metabolite of aflatoxin B1), as well as other aflatoxins, under competitive conditions. We determined optimal aflatoxin extraction conditions in terms of concentration, flow rate, temperature, and embedded particle amount as up to 25ng/mL for each species, 0.43mL/min, 7.0, 30°C, and 200mg, respectively. These multiclonal plastic antibodies showed imprinting efficiencies against ochratoxin A and aflatoxin M1 of 1.84 and 26.39, respectively, even under competitive conditions. Finally, we tested reusability, repeatability, reproducibility, and robustness of columns throughout inter- and intra-column variation studies. Copyright © 2016 Elsevier Ltd. All rights reserved.

Impact of the uranium (VI) speciation in mineralised urines on its extraction by calix[6]arene bearing hydroxamic groups used in chromatography columns.

PubMed

Baghdadi, S; Bouvier-Capely, C; Ritt, A; Peroux, A; Fevrier, L; Rebiere, F; Agarande, M; Cote, G

2015-11-01

Actinides determination in urine samples is part of the analyses performed to monitor internal contamination in case of an accident or a terrorist attack involving nuclear matter. Mineralisation is the first step of any of these analyses. It aims at reducing the sample volume and at destroying all organic compounds present. The mineralisation protocol is usually based on a wet ashing step, followed by actinides co-precipitation and a furnace ashing step, before redissolution and the quantification of the actinides by the appropriate techniques. Amongst the existing methods to perform the actinides co-precipitation, alkali-earth (typically calcium) precipitation is widely used. In the present work, the extraction of uranium(VI), plutonium(IV) and americium(III) from the redissolution solutions (called "mineralised urines") on calix[6]arene columns bearing hydroxamic groups was investigated as such an extraction is a necessary step before their determination by ICP-MS or alpha spectrometry. Difficulties were encountered in the transfer of uranium(VI) from raw to mineralised urines, with yield of transfer ranging between 0% and 85%, compared to about 90% for Pu and Am, depending on the starting raw urines. To understand the origin of such a difficulty, the speciation of uranium (VI) in mineralised urines was investigated by computer simulation using the MEDUSA software and the associated HYDRA database, compiled with recently published data. These calculations showed that the presence of phosphates in the "mineralised urines" leads to the formation of strong uranyl-phosphate complexes (such as UO2HPO4) which compete with the uranium (VI) extraction by the calix[6]arene bearing hydroxamic groups. The extraction constant of uranium (VI) by calix[6]arene bearing hydroxamic groups was determined in a 0.04 mol L(-1) sodium nitrate solution (logK=4.86±0.03) and implemented in an extraction model taking into account the speciation in the aqueous phase. This model allowed to simulate satisfactorily the experimental uranium extraction data and to support the preliminary conclusions about the role of the phosphates present in mineralised urines. These calculations also showed that the phosphate/calcium ratio is a key parameter as far as the efficiency of the uranium (VI) extraction by the calix[6]arene columns is concerned. It predicted that the addition of CaCl2 in mineralised urines would release uranium (VI) from phosphates by forming calcium (II)-phosphate complexes and thus facilitate the uranium (VI) extraction on calix[6]arene columns. These predictions were confirmed experimentally as the addition of 0.1 mol L(-1) CaCl2 to a mineralised urine containing naturally a high concentration of phosphate (typically 0.04 mol L(-1)) significantly increased the percentage of uranium (VI) extraction on the calix[6]arene columns. Copyright © 2015 Elsevier B.V. All rights reserved.

Surface micro-structuring of silicon by excimer-laser irradiation in reactive atmospheres

NASA Astrophysics Data System (ADS)

Pedraza, A. J.; Fowlkes, J. D.; Jesse, S.; Mao, C.; Lowndes, D. H.

2000-12-01

The formation mechanisms of cones and columns by pulsed-laser irradiation in reactive atmospheres were studied using scanning electron microscopy and profilometry. Deep etching takes place in SF6- and O2- rich atmospheres and consequently, silicon-containing molecules and clusters are released. Transport of silicon from the etched/ablated regions to the tip of columns and cones and to the side of the cones is required because both structures, columns and cones, protrude above the initial surface. The laser-induced micro-structure is influenced not only by the nature but also by the partial pressure of the reactive gas in the atmosphere. Irradiation in Ar following cone formation in SF6 produced no additional growth but rather melting and resolidification. Subsequent irradiation using again a SF6 atmosphere lead to cone restructuring and growth resumption. Thus the effects of etching plus re-deposition that produce column/cone formation and growth are clearly separated from the effects of just melting. On the other hand, irradiation continued in air after first performed in SF6 resulted in: (a) an intense etching of the cones and a tendency to transform them into columns; (b) growth of new columns on top of the existing cones and (c) filamentary nano-structures coating the sides of the columns and cones.

Pilot-Scale Test of Counter-Current Ion Exchange (CCIX) Using UOP IONSIV IE-911

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

Wester, Dennis W; Leugemors, Robert K; Taylor, Paul W

2001-09-24

A pilot-scale test of a moving-bed configuration of a UOP IONSIV? IE-911 ion-exchange column was performed over 17 days at Severn Trent Services facilities. The objectives of the test, in order of priority, were to determine if aluminosilicate precipitation caused clumping of IE-911 particles in the column, to observe the effect on aluminum-hydroxide precipitation of water added to a simulant-filled column, to evaluate the extent of particle attrition, and to measure the expansion of the mass-transfer zone under the influence of column pulsing. The IE-911 moved through the column with no apparent clumping during the test, although analytical results indicatemore » that little if any aluminosilicate precipitated onto the particles. A precipitate of aluminum hydroxide was not produced when water was added to the simulant-filled column, indicating that this upset scenario is probably of little concern. Particle-size distributions remained relatively constant with time and position in the column, indicating that particle attrition was not significant. The expansion of the mass-transfer zone could not be accurately measured because of the slow loading kinetics of the IE-911 and the short duration of the test; however, the information obtained indicates that back-mixing of sorbent is not extensive.« less

Review of controlled fusion research using laser heating.

NASA Technical Reports Server (NTRS)

Hertzberg, A.

1973-01-01

Development of methods for generating high laser pulse energy has stimulated research leading to new ideas for practical controlled thermonuclear fusion machines. A review is presented of some important efforts in progress, and two different approaches have been selected as examples for discussion. One involves the concept of very short pulse lasers with power output tailored, in time, to obtain a nearly isentropic compression of a deuterium-tritium pellet to very high densities and temperatures. A second approach utilizing long wavelength, long pulse, efficient gas lasers to heat a column of plasma contained in a solenoidal field is also discussed. The working requirements of the laser and various magnetic field geometries of this approach are described.

Rapid non-enzymatic extraction method for isolating PCR-quality camelpox virus DNA from skin.

PubMed

Yousif, A Ausama; Al-Naeem, A Abdelmohsen; Al-Ali, M Ahmad

2010-10-01

Molecular diagnostic investigations of orthopoxvirus (OPV) infections are performed using a variety of clinical samples including skin lesions, tissues from internal organs, blood and secretions. Skin samples are particularly convenient for rapid diagnosis and molecular epidemiological investigations of camelpox virus (CMLV). Classical extraction procedures and commercial spin-column-based kits are time consuming, relatively expensive, and require multiple extraction and purification steps in addition to proteinase K digestion. A rapid non-enzymatic procedure for extracting CMLV DNA from dried scabs or pox lesions was developed to overcome some of the limitations of the available DNA extraction techniques. The procedure requires as little as 10mg of tissue and produces highly purified DNA [OD(260)/OD(280) ratios between 1.47 and 1.79] with concentrations ranging from 6.5 to 16 microg/ml. The extracted CMLV DNA was proven suitable for virus-specific qualitative and, semi-quantitative PCR applications. Compared to spin-column and conventional viral DNA extraction techniques, the two-step extraction procedure saves money and time, and retains the potential for automation without compromising CMLV PCR sensitivity. Copyright (c) 2010 Elsevier B.V. All rights reserved.

[Effect of the ethanol extracts of starfish Asterias amurensis on the levels of serum IL-4 and IFN-γ in mice].

PubMed

He, Su-hui; Tang, Xiao-lei; Deng, Ye-feng; Chen, Zhang-quan

2011-11-01

To investigate the effect of the ethanol extracts of the starfish Asterias amurensis on the levels of serum IL-4 and IFN-γ in mice. The whole bodies of the starfish were chopped and extracted with ethanol. The ethanol extracts were chromatographed on silica gel column. The separating fractions of the ethanol extracts were intraperitoneally injected into mice, respectively. The levels of serum IL-4 and IFN-γ in mice were detected by ELISA. The ethanol extracts from the starfish were separated through silica gel column chromatography to obtain 8 fractions (I-VIII). The high levels of IL-4 and IFN-γ were produced in serum of the mice injected with fractions III and VIII of the ethanol extracts from the starfish Asterias amurensis. The fractions III and VIIII separated from the ethanol extracts of the starfish Asterias amurensis can stimulate the mice to produce high lelves of IL-4 and IFN-γ, which has the characteristic of natural kill T (NKT) cells activator. It is suggests that there is the active substance that can activate NKT cells in the starfish Asterias amurensis.

Water-compatible molecularly imprinted polymers for efficient direct injection on-line solid-phase extraction of ropivacaine and bupivacaine from human plasma.

PubMed

Cobb, Zoe; Sellergren, Börje; Andersson, Lars I

2007-12-01

Two novel molecularly imprinted polymers (MIPs) selected from a combinatorial library of bupivacaine imprinted polymers were used for selective on-line solid-phase extraction of bupivacaine and ropivacaine from human plasma. The MIPs were prepared using methacrylic acid as the functional monomer, ethylene glycol dimethacrylate as the cross-linking monomer and in addition hydroxyethylmethacrylate to render the polymer surface hydrophilic. The novel MIPs showed high selectivity for the analytes and required fewer and lower concentrations of additives to suppress non-specific adsorption compared with a conventional MIP. This enabled the development of an on-line system for direct extraction of buffered plasma. Selective extraction was achieved without the use of time-consuming solvent switch steps, and transfer of the analytes from the MIP column to the analytical column was carried out under aqueous conditions fully compatible with reversed-phase LC gradient separation of analyte and internal standard. The MIPs showed excellent aqueous compatibility and yielded extractions with acceptable recovery and high selectivity.

Laboratory Information Bulletin: Quantitation of Aflatoxin M1 in Bovine Milk by Liquid Chromatography with Fluorescence Detection.

PubMed

Vega, Victor A; Young, Michelle; Todd, Sarah

2016-01-01

An extraction for aflatoxin M1 from bovine milk samples is described. The samples were extracted by adding 10 mL acetonitrile to 10 g of sample. The extract was salted out with sodium chloride and magnesium sulfate to separate the water and acetonitrile. The organic layer was dried down and reconstituted in water before being subjected to an immunoaffinity column for cleanup. Once the analyte was isolated, quantitation was obtained by LC with fluorescence detection. LC/fluorescence parameters were optimized with an Agilent Poroshell 120 C18 LC column resulting in a 4 min run time. To test the procedure's robustness, three different kinds of matrixes were fortified at three different levels each. Whole milk, reduced fat milk, and skim milk samples were fortified at approximately 0.25, 0.5, and 1.0 μg/kg. Recoveries from all samples ranged from 70 to 100%. Confirmation was accomplished by injecting the samples in an ion trap mass spectrometer. The method presented here entails an extraction step followed by an immunoaffinity column clean-up that leads to fast analysis time and consistent recoveries with an uncertainty measurement of 10.5% and method detection limit of less than 0.011 μg/kg.

Rapid determination of polycyclic aromatic hydrocarbons in rainwater by liquid-liquid microextraction and LC with core-shell particles column and fluorescence detection.

PubMed

Vinci, Giuliana; Antonelli, Marta L; Preti, Raffaella

2013-02-01

Liquid-liquid microextraction coupled to LC with fluorescence detection for the determination of Environmental Protection Agency's 16 priority pollutant polycyclic aromatic hydrocarbons in rainwater has been developed. The optimization of the extraction method has involved several parameters, including the comparison between an ultrasonic bath and a magnetic stirrer as extractant apparatus, the choice of the extractant solvent, and the optimization of the extraction time. Liquid-liquid microextraction gave good results in terms of recoveries (from 73.6 to 102.8% in rainwater) and repeatability, with a very simple procedure and low solvent consumption. The reported chromatographic method uses a Core-Shell technology column, with particle size <3 μm instead of classical 5-μm particles column. The resulting backpressure was below 300 bar, allowing the use of a conventional HPLC system rather than the more expensive ultrahigh performance LC (UHPLC). An average decrease of 59% in run time and 75% in eluent consumption has been obtained, compared to classical HPLC methods, keeping good separation, sensitivity, and repeatability. The proposed conditions were successfully applied to the determinations of polycyclic aromatic hydrocarbons in genuine rainwater samples. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Detection of phytoconstituents in column fractions of n-hexane extract of Goldcrest honey exhibiting anti-Helicobacter pylori activity.

PubMed

Manyi-Loh, Christy E; Clarke, Anna M; Ndip, Roland N

2012-04-01

Alternative therapy for Helicobacter pylori eradication from natural products is gaining much attention. This study sought to isolate and characterize the fraction responsible for the antibacterial activity in Goldcrest (GC) n-hexane extract. Thin-layer chromatography (TLC) of the extract was carried out on Silica gel plates to determine the presence of chemical compounds, which were separated and partially purified by column chromatography. The obtained fractions GCCL, GCF2, GCF3 and GCF4 were tested for anti-H. pylori activity using the broth microdilution method. Volatile compounds in the active fractions were identified by gas chromatography-mass spectrometry (GC-MS) analysis. MINITAB was used for statistical analysis at 95% confidence interval. The best antibacterial activity was exhibited by GCF3 (5 mg/mL), which was composed of many compounds with known antimicrobial and antioxidant properties. A total of 16 volatile compounds were identified from fractions GCF2, GCF3 and GCF4 into the following families; alcohol, ketone, aliphatic acid, benzene compound, hydrocarbon, furan and pyran derivatives. The demonstration of antibacterial activity by the column fractions of GC n-hexane extract may provide new lead molecules that could serve as selective agents for H. pylori chemotherapy and control. Copyright © 2012 IMSS. Published by Elsevier Inc. All rights reserved.

A Simplified Method for Sampling and Analysis of High Volume Surface Water for Organic Contaminants Using XAD-2

USGS Publications Warehouse

Datta, S.; Do, L.V.; Young, T.M.

2004-01-01

A simple compressed-gas driven system for field processing and extracting water for subsequent analyses of hydrophobic organic compounds is presented. The pumping device is a pneumatically driven pump and filtration system that can easily clarify at 4L/min. The extraction device uses compressed gas to drive filtered water through two parallel XAD-2 resin columns, at about 200 mL/min. No batteries or inverters are required for water collection or processing. Solvent extractions were performed directly in the XAD-2 glass columns. Final extracts are cleaned-up on Florisil cartridges without fractionation and contaminants analyzed by GC-MS. Method detection limits (MDLs) and recoveries for dissolved organic contaminants, polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs) and pesticides are reported along with results of surface water analysis for the San Francisco Bay, CA.

Bioactive phenolic derivatives from Acaena splendens methanol extract.

PubMed

Backhouse, N; Delporte, C; Negrete, R; Feliciano, S A San; López-Pérez, J L

2002-09-01

Acaena splendens H. et A. has been used in Chilean folk medicine for the treatment of fever and inflammation. A description of the in vivo reduction of bacterial pyrogen-induced fever in rabbits and carrageenan-induced paw oedema in guinea pigs is presented. The methanol extract named ME-1, obtained after succesive extractions with petroleum ether and dichloromethane, showed a strong antipyretic action (45.7% of effect), though the antiinflammatory activity was only observed after submitting this extract to column fractionation, giving a crude mixture of flavonoids named C4 with both activities (55.7% and 98.9% of antiinflammatory and antipyretic effect respectively at a dose of 600 mg/kg). The bioassay-guided fractionation by column chromatography afforded the active fraction, which contained (-,-)-epicatechin, tiliroside, 7-O-acetyl-3-O-beta-D-glucosyl-kaempferol and 7-beta-D-glucosyloxy-5-hydroxy-chromone. Copyright 2002 John Wiley & Sons, Ltd.

Ultrasound-assisted analyte extraction for the determination of sulfate and elemental sulfur in zinc sulfide by different liquid chromatography techniques.

PubMed

Dash, K; Thangavel, S; Krishnamurthy, N V; Rao, S V; Karunasagar, D; Arunachalam, J

2005-04-01

The speciation and determination of sulfate (SO4(2-)) and elemental sulfur (S degree) in zinc sulfide (ZnS) using ion-chromatography (IC) and reversed-phase liquid chromatography (RPLC) respectively is described. Three sample pretreatment approaches were employed with the aim of determining sulfate: (i) conventional water extraction of the analyte; (ii) solid-liquid aqueous extraction with an ultrasonic probe; and (iii) elimination of the zinc sulfide matrix via ion-exchange dissolution (IED). The separation of sulfate was carried out by an anion-exchange column (IonPac AS17), followed by suppressed conductivity detection. Elemental sulfur was extracted ultrasonically from the acid treated sample solution into chloroform and separated on a reversed phase HPLC column equipped with a diode array detector (DAD) at 264 nm. The achievable solid detection limits for sulfate and sulfur were 35 and 10 microg g(-1) respectively.

Polytetrafluorethylene film-based liquid-three phase micro extraction coupled with differential pulse voltammetry for the determination of atorvastatin calcium.

PubMed

Ensafi, Ali A; Khoddami, Elaheh; Rezaei, Behzad

2013-01-01

In this paper, we describe a new combination method based on polytetrafluorethylene (PTFE) film-based liquid three-phase micro extraction coupled with differential pulse voltammetry (DPV) for the micro extraction and quantification of atorvastatin calcium (ATC) at the ultra-trace level. Different factors affecting the liquid-three phases micro extraction of atorvastatin calcium, including organic solvent, pH of the donor and acceptor phases, concentration of salt, extraction time, stirring rate and electrochemical factors, were investigated, and the optimal extraction conditions were established. The final stable signal was achieved after a 50 min extraction time, which was used for analytical applications. An enrichment factor of 21 was achieved, and the relative standard deviation (RSD) of the method was 4.5% (n = 4). Differential pulse voltammetry exhibited two wide linear dynamic ranges of 20.0-1000.0 pmol L(-1) and 0.001-11.0 µmol L(-1) of ATC. The detection limit was found to be 8.1 pmol L(-1) ATC. Finally, the proposed method was used as a new combination method for the determination of atorvastatin calcium in real samples, such as human urine and plasma.

RF extraction issues in the relativistic klystron amplifiers

NASA Astrophysics Data System (ADS)

Serlin, Victor; Friedman, Moshe; Lampe, Martin; Hubbard, Richard F.

1994-05-01

Relativistic klystron amplifiers (RKAs) were successfully operated at NRL in several frequency regimes and power levels. In particular, an L-band RKA was optimized for high- power rf extraction into the atmosphere and an S-band RKA was operated, both in a two-beam and a single-beam configuration. At L-band the rf extraction at maximum power levels (>= 15 GW) was hindered by pulse shortening and poor repeatability. Preliminary investigation showed electron emission in the radiating horn, due to very high voltages associated with the multi-gigawatt rf power levels. This electron current constituted an electric load in parallel with the radiating antenna, and precipitated the rf pulse collapse. At S-band the peak extracted power reached 1.7 GW with power efficiency approximately 50%. However, pulse shortening limited the duration to approximately 50 nanoseconds. The new triaxial RKA promises to solve many of the existing problems.

Rapid trace level determination of sulfonamide residues in honey with online extraction using short C-18 column by high-performance liquid chromatography with fluorescence detection.

PubMed

Sajid, Muhammad; Na, Na; Safdar, Muhammad; Lu, Xin; Ma, Lin; He, Lan; Ouyang, Jin

2013-11-01

A sensitive and inexpensive quantification method with online extraction using a short C-18 column for sulfonamide residues in honey by high performance liquid chromatography with fluorescence detector was developed and validated. In sample preparation, acid hydrolysis was used to break the N-glycoside bond between the honey sugar and sulfonamide drugs and derivatization of sulfonamide residues with fluorescamine was conducted at pH 3.5 using a citrate buffer (0.5M) in the honey matrix. The chromatography was carried out on Zorbax Extended C-18 (250mm×4.6mm; 5μm) column, using a mixture of acetonitrile and an acetate buffer (pH 4.50, 20mM) as a mobile phase. A Zorbax Extended C-18 (12mm×4.6mm; 5μm) column was used for online extraction of fifteen sulfonamide residues from honey sample with the help of a two position valve. The limit of quantification of sulfonamide residues in honey was less than 3ngg(-1), and the percentage recovery of study compounds in spiked honey sample was from 80% for sulfacetamide to 100% of sulfachloropyridazine. The developed method has excellent linearity for all studied sulfonamides with a correlation coefficient 0.993. Copyright © 2013 Elsevier B.V. All rights reserved.

Anti-inflammatory effect of bee pollen ethanol extract from Cistus sp. of Spanish on carrageenan-induced rat hind paw edema.

PubMed

Maruyama, Hiroe; Sakamoto, Takashi; Araki, Yoko; Hara, Hideaki

2010-06-23

Bee pollen, a honeybee product, is the feed for honeybees prepared themselves by pollens collecting from plants and has been consumed as a perfect food in Europe, because it is nutritionally well balanced. In this study, we aimed to investigate the anti-inflammatory effect of bee pollen from Cistus sp. of Spanish origin by a method of carrageenan-induced paw edema in rats, and to investigate the mechanism of anti-inflammatory action and also to elucidate components involved in bee pollen extracted with ethanol. The bee pollen bulk, its water extract and its ethanol extract were administered orally to rats. One hour later, paw edema was produced by injecting of 1% solution of carrageenan, and paw volume was measured before and after carrageenan injection up to 5 h. The ethanol extract and water extract were measured COX-1 and COX-2 inhibitory activities using COX inhibitor screening assay kit, and were compared for the inhibition of NO production in LPS-stimulated RAW 264.7 cells. The constituents of bee pollen were purified from the ethanol extract subjected to silica gel or LH-20 column chromatography. Each column chromatography fractions were further purified by repeated ODS or silica gel column chromatography. The bee pollen bulk mildly suppressed the carrageenan-induced paw edema and the water extract showed almost no inhibitory activity, but the ethanol extract showed relatively strong inhibition of paw edema. The ethanol extract inhibited the NO production and COX-2 but not COX-1 activity, but the water extract did not affect the NO production or COX activities. Flavonoids were isolated and purified from the ethanol extract of bee pollen, and identified at least five flavonoids and their glycosides. It is suggested that the ethanol extract of bee pollen show a potent anti-inflammatory activity and its effect acts via the inhibition of NO production, besides the inhibitory activity of COX-2. Some flavonoids included in bee pollen may partly participate in some of the anti-inflammatory action. The bee pollen would be beneficial not only as a dietary supplement but also as a functional food.

Anti-inflammatory effect of bee pollen ethanol extract from Cistus sp. of Spanish on carrageenan-induced rat hind paw edema

PubMed Central

2010-01-01

Background Bee pollen, a honeybee product, is the feed for honeybees prepared themselves by pollens collecting from plants and has been consumed as a perfect food in Europe, because it is nutritionally well balanced. In this study, we aimed to investigate the anti-inflammatory effect of bee pollen from Cistus sp. of Spanish origin by a method of carrageenan-induced paw edema in rats, and to investigate the mechanism of anti-inflammatory action and also to elucidate components involved in bee pollen extracted with ethanol. Methods The bee pollen bulk, its water extract and its ethanol extract were administered orally to rats. One hour later, paw edema was produced by injecting of 1% solution of carrageenan, and paw volume was measured before and after carrageenan injection up to 5 h. The ethanol extract and water extract were measured COX-1 and COX-2 inhibitory activities using COX inhibitor screening assay kit, and were compared for the inhibition of NO production in LPS-stimulated RAW 264.7 cells. The constituents of bee pollen were purified from the ethanol extract subjected to silica gel or LH-20 column chromatography. Each column chromatography fractions were further purified by repeated ODS or silica gel column chromatography. Results The bee pollen bulk mildly suppressed the carrageenan-induced paw edema and the water extract showed almost no inhibitory activity, but the ethanol extract showed relatively strong inhibition of paw edema. The ethanol extract inhibited the NO production and COX-2 but not COX-1 activity, but the water extract did not affect the NO production or COX activities. Flavonoids were isolated and purified from the ethanol extract of bee pollen, and identified at least five flavonoids and their glycosides. Conclusions It is suggested that the ethanol extract of bee pollen show a potent anti-inflammatory activity and its effect acts via the inhibition of NO production, besides the inhibitory activity of COX-2. Some flavonoids included in bee pollen may partly participate in some of the anti-inflammatory action. The bee pollen would be beneficial not only as a dietary supplement but also as a functional food. PMID:20573205

Simultaneous achiral-chiral analysis of pharmaceutical compounds using two-dimensional reversed phase liquid chromatography-supercritical fluid chromatography.

PubMed

Venkatramani, C J; Al-Sayah, Mohammad; Li, Guannan; Goel, Meenakshi; Girotti, James; Zang, Lisa; Wigman, Larry; Yehl, Peter; Chetwyn, Nik

2016-02-01

A new interface was designed to enable the coupling of reversed phase liquid chromatography (RPLC) and supercritical fluid chromatography (SFC). This online two-dimensional chromatographic system utilizing RPLC in the first dimension and SFC in the second was developed to achieve simultaneous achiral and chiral analysis of pharmaceutical compounds. The interface consists of an eight-port, dual-position switching valve with small volume C-18 trapping columns. The peaks of interest eluting from the first RPLC dimension column were effectively focused as sharp concentration pulses on small volume C-18 trapping column/s and then injected onto the second dimension SFC column. The first dimension RPLC separation provides the achiral purity result, and the second dimension SFC separation provides the chiral purity result (enantiomeric excess). The results are quantitative enabling simultaneous achiral, chiral analysis of compounds. The interface design and proof of concept demonstration are presented. Additionally, comparative studies to conventional SFC and case studies of the applications of 2D LC-SFC in pharmaceutical analysis is presented. Copyright © 2015 Elsevier B.V. All rights reserved.

Effect of Pulsed Ultraviolet Light and High Hydrostatic Pressure on the Antigenicity of Almond Protein Extracts.

USDA-ARS?s Scientific Manuscript database

The efficacy of pulsed ultraviolet light (PUV) and high hydrostatic pressure (HHP) on reducing the IgE binding to the almond extracts, was studied using SDS-PAGE, Western Blot, and ELISA probed with human plasma containing IgE antibodies to almond allergens, and a polyclonal antibody against almond ...

Analysis of Pulsed Airborne Lidar Measurements of Atmospheric CO2 Column Absorption from 3-13 km Altitudes

NASA Technical Reports Server (NTRS)

Abshire, James B.; Weaver, Clark J.; Riris, Haris; Mao, Jianping; Sun, Xiaoli; Allan, Graham R.; Hasselbrack, William; Browell, Edward V.

2011-01-01

We have developed a pulsed lidar technique for measuring the tropospheric CO2 concentrations as a candidate for NASA's ASCENDS space mission [1]. It uses two pulsed laser transmitters allowing simultaneous measurement of a CO2 absorption line in the 1575 nm band, O2 extinction in the Oxygen A-band, surface height and backscatter profile. The lasers are precisely stepped in wavelength across the CO2 line and an O2 line region during the measurement. The direct detection receiver measures the energies of the laser echoes from the surface along with the range profile of scattering in the path. The column densities for the CO2 and O2 gases are estimated from the ratio of the on- and off-line signals via the integrated path differential absorption (IPDA) technique. The time of flight of the laser pulses is used to estimate the height of the scattering surface and to reject laser photons scattered in the atmosphere. We developed an airborne lidar to demonstrate an early version of the CO2 measurement from the NASA Glenn Lear-25 aircraft. The airborne lidar stepped the pulsed laser's wavelength across the selected CO2 line with 20 wavelength steps per scan. The line scan rate is 450 Hz, the laser pulse widths are 1 usec, and laser pulse energy is 24 uJ. The time resolved laser backscatter is collected by a 20 cm telescope, detected by a NIR photomultiplier and is recorded on every other reading by a photon counting system [2]. During August 2009 we made a series of 2.5 hour long flights and measured the atmospheric CO2 absorption and line shapes using the 1572.33 nm CO2 line. Measurements were made at stepped altitudes from 3-13 km over locations in the US, including the SGP ARM site in Oklahoma, central Illinois, north-eastern North Carolina, and over the Chesapeake Bay and the eastern shore of Virginia. Although the received signal energies were weaker than expected for ASCENDS, clear CO2 line shapes were observed at all altitudes, and some measurements were made through thin clouds. The Oklahoma and east coast flights were coordinated with a LaRC/ITT CO2 lidar on the LaRC UC-12 aircraft, and in-situ measurements were made using its CO2 sensor and radiosondes. We have conducted an analysis of the ranging and IPDA lidar measurements from these four flights. Most flights had 5-6 altitude steps with 200-300 seconds of recorded measurements per step. We used a cross-correlation approach to process the laser echo records. This was used to estimate the range to the scattering surface, to define the edges of the laser pulses and to determine echo pulse energy at each wavelength. We used a minimum mean square approach to fit an instrument response function and to solve for the best-fit CO2 absorption line shape. We then calculated the differential optical depth (DOD) of the fitted CO2 line. We computed its statistics at the various altitude steps, and compare them to the DODs calculated from spectroscopy based on HITRAN 2008 and the column conditions calculated from the airborne in-situ readings. The results show the lidar and in-situ measurements have very similar DOD change with altitude and greater than 10 segments per flight where the scatter in the lidar measurements are less than or equal to 1ppm. We also present the results from subsequent CO2 column absorption measurements, which were made with stronger detected signals during three flights on the NASA DC-8 over the southwestern US in during July 2010.

Column chromatography as a useful step in purification of diatom pigments.

PubMed

Tokarek, Wiktor; Listwan, Stanisław; Pagacz, Joanna; Leśniak, Piotr; Latowski, Dariusz

2016-01-01

Fucoxanthin, diadinoxanthin and diatoxanthin are carotenoids found in brown algae and most other heterokonts. These pigments are involved in photosynthetic and photoprotective reactions, and they have many potential health benefits. They can be extracted from diatom Phaeodactylum tricornutum by sonication, extraction with chloroform : methanol and preparative thin layer chromatography. We assessed the utility of an additional column chromatography step in purification of these pigments. This novel addition to the isolation protocol increased the purity of fucoxanthin and allowed for concentration of diadinoxanthin and diatoxanthin before HPLC separation. The enhanced protocol is useful for obtaining high purity pigments for biochemical studies.

Staring at 4U 1909+07 with Suzaku (Research Note)

NASA Technical Reports Server (NTRS)

Fuerst, F.; Pottschmidt, K.; Kreykenbohm, I.; Mueller, S.; Kuehnel, M.; Wilms, J.; Rothschild, R. E.

2012-01-01

We present an analysis of the neutron star High Mass X-ray Binary (HMXB) 4U 1909+07 mainly based on Suzaku data. We extend the pulse period evolution, which behaves in a random-walk like manner, indicative of direct wind accretion. Studying the spectral properties of 4U 1909+07 between 0.5 to 90keV we find that a power-law with an exponential cutoff can describe the data well, when additionally allowing for a blackbody or a partially covering absorber at low energies. We find no evidence for a cyclotron resonant scattering feature (CRSF), a feature seen in many other neutron star HMXBs sources. By performing pulse phase resolved spectroscopy we investigate the origin of the strong energy dependence of the pulse profile, which evolves from a broad two-peak profile at low energies to a profile with a single, narrow peak at energies above 20keV. Our data show that it is very likely that a higher folding energy in the high energy peak is responsible for this behavior. This in turn leads to the assumption that we observe the two magnetic poles and their respective accretion columns at different phases, and that these accretions column have slightly different physical conditions.

Isolation of atropine and scopolamine from plant material using liquid-liquid extraction and EXtrelut® columns.

PubMed

Śramska, Paula; Maciejka, Artur; Topolewska, Anna; Stepnowski, Piotr; Haliński, Łukasz P

2017-02-01

Tropane alkaloids are toxic secondary metabolites produced by Solanaceae plants. Among them, plants from Datura genus produce significant amounts of scopolamine and hyoscyamine; the latter undergoes racemization to atropine during isolation. Because of their biological importance, toxic properties and commonly reported food and animal feed contamination by different Datura sp. organs, there is a constant need for reliable methods for the analysis of tropane alkaloids in many matrices. In the current study, three extraction and sample-clean up procedures for the determination of scopolamine and atropine in plant material were compared in terms of their effectiveness and repeatability. Standard liquid-liquid extraction (LLE) and EXtrelut ® NT 3 columns were used for the sample clean-up. Combined ultrasound-assisted extraction and 24h static extraction using ethyl acetate, followed by multiple LLE steps was found the most effective separation method among tested. However, absolute extraction recovery was relatively low and reached 45-67% for atropine and 52-73% for scopolamine, depending on the compound concentration. The same method was also the most effective one for the isolation of target compounds from Datura stramonium leaves. EXtrelut ® columns, on the other hand, displayed relatively low effectiveness in isolating atropine and scopolamine from such a complex matrix and hence could not be recommended. The most effective method was also applied to the extraction of alkaloids from roots and stems of D. stramonium. Quantitative analyses were performed using validated method based on gas chromatography with flame ionization detector (GC-FID). Based on the results, the importance of the proper selection of internal standards in the analysis of tropane alkaloids was stressed out. Copyright © 2016 Elsevier B.V. All rights reserved.

Acaricidal activity of petroleum ether extract of neem (Azadirachta indica) oil and its four fractions separated by column chromatography against Sarcoptes scabiei var. cuniculi larvae in vitro.

PubMed

Deng, Yunxia; Shi, Dongxia; Yin, Zhongqiong; Guo, Jianhong; Jia, Renyong; Xu, Jiao; Song, Xu; Lv, Cheng; Fan, Qiaojia; Liang, Xiaoxia; Shi, Fei; Ye, Gang; Zhang, Wei

2012-04-01

The petroleum ether extract of neem oil and its four fractions separated by column chromatography was diluted at different concentrations with liquid paraffin. The acaricidal bioassay was conducted using a dipping method. The results indicated that the median lethal concentration (LC50) of the petroleum ether extract (at the concentration of 500.0ml/l) was 70.9ml/l, 24h after treatment. At concentrations of 500.0, 250.0, 125.0, 62.5 and 31.2ml/l, the median lethal times (LT50) of the petroleum ether extract were 8.7, 8.8, 10.8, 11.5 and 13.1h, respectively. Thin-layer chromatography (TLC) showed that the petroleum ether extract of neem oil separated into four fractions (F1-F4). Acaricidal activity of 68.3% and 100.0% in the F2 and F4 was confirmed. These results suggest that petroleum ether extracts of neem oil and its four fractions possess useful acaricidal activity in vitro. Copyright © 2012 Elsevier Inc. All rights reserved.

Rapid determination of benzo(a)pyrene in roasted coffee and coffee brew by high-performance liquid chromatography with fluorescence detection

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

de Kruijf, N.; Schouten, T.; van der Stegen, G.H.D.

A rapid and reliable analytical method is presented for the determination of trace amounts of benzo(a)pyrene in roasted coffee, coffee brew, and spent grounds. Roasted coffee and spent grounds were extracted with acetone, followed by saponification and cyclohexane extraction. Coffee brew was extracted three times with cyclohexane, and the combined extracts were purified by chromatography on a silica gel column. The extracts were analyzed by HPLC with a 5-..mu..m Vydac reversed-phase 201 TPB 5 column and fluorescence detection under isocratic conditions. The benzo(a)pyrene levels in 55 roasted coffee samples, commercially available in the Netherlands, ranged from not detectable (<0.1 ..mu..g/kg)more » to 0.5 ..mu..g/kg. Coffee brews were prepared by two different methods from an over-roasted coffee sample with an elevated benzo(a)pyrene level of 2 ..mu..g/kg. These brews yielded benzo(a)pyrene contents of approximately 1 ng/L, indicating benzo(a)pyrene extraction yields of about 1% for both coffee preparation methods.« less

Quantitative determination of 5-hydroxy-N-methylpyrrolidone in urine for biological monitoring of N-methylpyrrolidone exposure.

PubMed

Ligocka, D; Lison, D; Haufroid, V

2002-10-05

The aim of this work was to validate a sensitive method for quantitative analysis of 5-hydroxy-N-methylpyrrolidone (5-HNMP) in urine. This compound has been recommended as a marker for biological monitoring of N-methylpyrrolidone (NMP) exposure. Different solvents and alternative methods of extraction including liquid-liquid extraction (LLE) on Chem Elut and solid-phase extraction (SPE) on Oasis HLB columns were tested. The most efficient extraction of 5-HNMP in urine was LLE with Chem Elut columns and dichloromethane as a solvent (consistently 22% of recovery). The urinary extracts were derivatized by bis(trimethylsilyl)trifluoroacetamide and analysed by gas chromatography-mass spectrometry (GC-MS) with tetradeutered 5-HNMP as an internal standard. The detection limit of this method is 0.017 mg/l urine with an intraassay precision of 1.6-2.6%. The proposed method of extraction is simple and reproducible. Four different m/z signal ratios of TMS-5-HNMP and tetralabelled TMS-5-HNMP have been validated and could be indifferently used in case of unexpected impurities from urine matrix. Copyright 2002 Elsevier Science B.V.

Comparison of two new generation pulse oximeters with arterial oxygen saturation in critically ill children.

PubMed

Jose, Bipin; Lodha, Rakesh; Kabra, S K

2014-12-01

To compare the performance of two new generation pulse oximeters, one with enhanced signal extraction technology (SET) and other without enhanced SET in detecting hypoxemia and to correlate it with arterial blood gas analysis. Forty-eight patients, admitted to pediatric intensive care unit (PICU) of a teritiary care teaching hospital in India for critical care and support during the study period, who had an arterial catheter in situ were included. Children with those disease conditions known to interfere with pulse oximetry and blood gas analysis were excluded.184 set of observations were made during the study period. Each set had oxygen saturation (SpO2) measured from both the pulse oximeters and the corresponding arterial oxygen saturation (SaO2). The values were compared for occurrence of true and false alarms during periods of normal BP, hypotension and varying degrees of hypoxia. The mean arterial SaO2 in the study was 94.4 % ± 4.9. The mean SpO2 recorded in conventional and enhanced signal extraction technology (SET) pulse oximeters were 94.9 % ± 4.5 and 97.2 % ± 4.7 respectively. Enhanced signal extraction technology pulse oximeter detected 4/27 (15 %) of true hypoxemic events and 1 event was a false alarm. Conventional pulse oximeter detected 11/27 (41 %) true hypoxemic events but recorded 6 false alarms. Both pulse oximeters were not found to be performing satisfactorily in picking up hypoxemia in the study. There was good correlation with mean SpO2 from pulse oximeters and arterial SaO2. The reliability of pulse oximetry decreases with worsening hypoxemia and hypotension, and the sensitivity for picking up hypoxemia can be as low as 15 %.

2-Micron Triple-Pulse Integrated Path Differential Absorption Lidar Development for Simultaneous Airborne Column Measurements of Carbon Dioxide and Water Vapor in the Atmosphere

NASA Technical Reports Server (NTRS)

Singh, Upendra N.; Petros, Mulugeta; Refaat, Tamer F.; Yu, Jirong

2016-01-01

For more than 15 years, NASA Langley Research Center (LaRC) has contributed in developing several 2-micron carbon dioxide active remote sensors using the DIAL technique. Currently, an airborne 2-micron triple-pulse integrated path differential absorption (IPDA) lidar is under development at NASA LaRC. This paper focuses on the advancement of the 2-micron triple-pulse IPDA lidar development. Updates on the state-of-the-art triple-pulse laser transmitter will be presented including the status of wavelength control, packaging and lidar integration. In addition, receiver development updates will also be presented, including telescope integration, detection systems and data acquisition electronics. Future plan for IPDA lidar system for ground integration, testing and flight validation will be presented.

Isolation and purification of diastereoisomeric flavonolignans from silymarin by binary-column recycling preparative high-performance liquid chromatography.

PubMed

Zhao, Weiquan; Yang, Guang; Zhong, Fanyi; Yang, Nan; Zhao, Xin; Qi, Yunpeng; Fan, Guorong

2014-09-01

Silymarin extracted from Silybum marianum (L.) Gaertn consists of a large number of flavonolignans, of which diastereoisomeric flavonolignans including silybin A and silybin B, and isosilybin A and isosilybin B are the main bioactive components, whose preparation from the crude extracts is still a difficult task. In this work, binary-column recycling preparative high-performance liquid chromatography systems without sample loop trapping, where two columns were switched alternately via one or two six-port switching valves, were established and successfully applied to the isolation and purification of the four diastereoisomeric flavonolignans from silymarin. The proposed system showed significant advantages over conventional preparative high-performance liquid chromatography with a single column in increasing efficiency and reducing the cost. To obtain the same amounts of products, the proposed system spends only one tenth of the time that the conventional system spends, and needs only one eleventh of the solvent that the conventional system consumes. Using the proposed system, the four diastereoisomers were successfully isolated from silymarin with purities over 98%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Rapid determination of five antibiotic residues in swine wastewater by online solid-phase extraction-high performance liquid chromatography-tandem mass spectrometry.

PubMed

Tagiri-Endo, Misako; Suzuki, Shigeru; Nakamura, Tomoyuki; Hatakeyama, Takashi; Kawamukai, Kazuo

2009-02-01

A simple and quick online solid-phase extraction (SPE) coupled to liquid chromatography (LC)/tandem mass spectrometry (MS/MS) for the determination of the five antibiotics (florfenicol, FF; lincomycin, LCM; oxytetracyclin, OTC; tylosin, TS; valnemulin, VLM) in swine wastewater has been developed. After filtration, aliquots (100 microl) of wastewater samples were directly injected to a column-switching LC system. Some matrix interference was removed by washing up SPE column with 0.2% formic acid solution and acetonitrile. Antibiotics eluted from SPE column were separated on analytical column by converting switching valve and were detected by MS/MS. Calibration curves using the method of standard addition had very good correlation coefficients (r > 0.99) in the range of 0.1 to 2 ng/ml. The intra-day precision of the method was less than 12% and the inter-day precision was between 6 to 17%. The detection limits were 0.01-0.1 ng/ml. When this method was applied to wastewater samples in swine facilities, four compounds (LCM, OTC, TS, and VLM) were detected.

Pulsed Lidar Measurements of Atmospheric CO2 Column Concentration in the ASCENDS 2014 Airborne Campaign

NASA Astrophysics Data System (ADS)

Abshire, J. B.; Ramanathan, A. K.; Mao, J.; Riris, H.; Allan, G. R.; Hasselbrack, W. E.; Chen, J. R.

2015-12-01

We report progress in demonstrating a pulsed, wavelength-resolved IPDA lidar technique for measuring the tropospheric CO2 concentrations as a candidate for NASA's ASCENDS mission. The CO2 lidar flies on NASA's DC-8 aircraft and measures the atmospheric backscatter profiles and shape of the 1572.33 nm absorption line by using 30 wavelength samples distributed across the lube. Our post-flight analysis estimates the lidar range and pulse energies at each wavelength 10 times per second. The retrievals solve for the optimum CO2 absorption line shape and the column average CO2 concentrations using radiative transfer calculations based on HITRAN, the aircraft altitude, range to the scattering surface, and the atmospheric conditions. We compare these to CO2 concentrations sampled by in-situ sensors on the aircraft. The number of wavelength samples can be reduced in the retrievals. During the ASCENDS airborne campaign in 2013 two flights were made in February over snow in the Rocky Mountains and the Central Plains allowing measurement of snow-covered surface reflectivity. Several improvements were made to the lidar for the 2014 campaign. These included using a new step-locked laser diode source, and incorporating a new HgCdTe APD detector and analog digitizer into the lidar receiver. Testing showed this detector had higher sensitivity, analog response, and a more linear dynamic range than the PMT detector used previously. In 2014 flights were made in late August and early September over the California Central Valley, the redwood forests along the California coast, two desert areas in Nevada and California, and two flights above growing agriculture in Iowa. Two flights were also made under OCO-2 satellite ground tracks. Analyses show the retrievals of lidar range and CO2 column absorption, and mixing ratio worked well when measuring over topography with rapidly changing height and reflectivity, and through thin clouds and aerosol scattering. The lidar measurements clearly show the decrease in CO2 concentration over growing cropland in Iowa. In several flights the agreement of the lidar with the column average concentration was < 1ppm, with standard deviation of 0.9 ppm. A summary of these results will be presented.

Dynamic fractionation of trace metals in soil and sediment samples using rotating coiled column extraction and sequential injection microcolumn extraction: a comparative study.

PubMed

Rosende, Maria; Savonina, Elena Yu; Fedotov, Petr S; Miró, Manuel; Cerdà, Víctor; Wennrich, Rainer

2009-09-15

Dynamic fractionation has been recognized as an appealing alternative to conventional equilibrium-based sequential extraction procedures (SEPs) for partitioning of trace elements (TE) in environmental solid samples. This paper reports the first attempt for harmonization of flow-through dynamic fractionation using two novel methods, the so-called sequential injection microcolumn (SIMC) extraction and rotating coiled column (RCC) extraction. In SIMC extraction, a column packed with the solid sample is clustered in a sequential injection system, while in RCC, the particulate matter is retained under the action of centrifugal forces. In both methods, the leachants are continuously pumped through the solid substrates by the use of either peristaltic or syringe pumps. A five-step SEP was selected for partitioning of Cu, Pb and Zn in water soluble/exchangeable, acid-soluble, easily reducible, easily oxidizable and moderately reducible fractions from 0.2 to 0.5 g samples at an extractant flow rate of 1.0 mL min(-1) prior to leachate analysis by inductively coupled plasma-atomic emission spectrometry. Similarities and discrepancies between both dynamic approaches were ascertained by fractionation of TE in certified reference materials, namely, SRM 2711 Montana Soil and GBW 07311 sediment, and two real soil samples as well. Notwithstanding the different extraction conditions set by both methods, similar trends of metal distribution were in generally found. The most critical parameters for reliable assessment of mobilizable pools of TE in worse-case scenarios are the size-distribution of sample particles, the density of particles, the content of organic matter and the concentration of major elements. For reference materials and a soil rich in organic matter, the extraction in RCC results in slightly higher recoveries of environmentally relevant fractions of TE, whereas SIMC leaching is more effective for calcareous soils.

Validation of double-pulse 1572 nm integrated path differential absorption lidar measurement of carbon dioxide

NASA Astrophysics Data System (ADS)

Du, Juan; Liu, Jiqiao; Bi, Decang; Ma, Xiuhua; Hou, Xia; Zhu, Xiaolei; Chen, Weibiao

2018-04-01

A ground-based double-pulse 1572 nm integrated path differential absorption (IPDA) lidar was developed for carbon dioxide (CO2) column concentrations measurement. The lidar measured the CO2 concentrations continuously by receiving the scattered echo signal from a building about 1300 m away. The other two instruments of TDLAS and in-situ CO2 analyzer measured the CO2 concentrations on the same time. A CO2 concentration measurement of 430 ppm with 1.637 ppm standard error was achieved.

Heat integrated ethanol dehydration flowsheets

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

Hutahaean, L.S.; Shen, W.H.; Brunt, V. Van

1995-04-01

zA theoretical evaluation of heat-integrated heterogeneous-azeotropic ethanol-water distillation flowsheets is presented. Simulations of two column flowsheets using several different hydrocarbon entrainers reveal a region of potential heat integration and substantial reduction in operating energy. In this paper, methods for comparing hydrocarbon entrainers are shown. Two aspects of entrainers are related to operating and capital costs. The binary azeotropic composition of the entrainer-ethanol mixture is related to the energy requirements of the flowsheet. A temperature difference in the azeotrophic column is related to the size of the column and overall process staging requirements. Although the hydrophobicity of an entrainer is essentialmore » for specification of staging in the dehydration column, no substantial increase in operating energy results from an entrainer that has a higher water content. Likewise, liquid-liquid equilibria between several entrainer-ethanol-water mixtures have no substantial effect on either staging or operation. Rather, increasing the alcohol content of the entrainer-ethanol azeotrope limits its recovery in the dehydration column, and increases the recycle and reflux streams. These effects both contribute to increasing the separation energy requirements and reducing the region of potential heat integration. A cost comparison with a multieffect extractive distillation flowsheet reveals that the costs are comparable; however, the extractive distillation flowsheet is more cost effective as operating costs increase.« less

Simultaneous determination of dextrose, sucrose, maltose, and lactose in sausage products by liquid chromatography.

PubMed

Ali, M S

1988-01-01

A liquid chromatographic (LC) method for the simultaneous determination of dextrose, sucrose, maltose, and lactose in sausage products has been developed. Dextrose, sucrose, maltose, and lactose are extracted from comminuted meat products with 52% ethanol. After filtration, the extracts are purified by passing them through a C18 Sep-Pak cartridge and 2 ion exchange resin Econo-columns in series. After concentration and filtration, extracts are analyzed by LC using a normal phase amino column and a differential refractometer detector. Homogeneously ground samples of cooked and fresh sausages are fortified with dextrose, sucrose, maltose, and lactose at 4 different concentrations. Average recovery for dextrose, sucrose, maltose, and lactose at all 4 levels of fortification was greater than 80% with a coefficient of variation less than 10%.

Study of the Anatomy of the X-Ray and Neutron Production Scaling Laws in the Plasma Focus (Particle Energy Spectrum and Optimization Criteria).

DTIC Science & Technology

1979-11-01

plasma focus operations have been experimentally analyzed in terms of (A) The fine structure of the axial-current channel during maximum of compression. (B) Correlation coefficient, for neutron yield n (by D2 discharges) and the multiplicity of the electron beam pulses; (C) Different values of the electrode voltage. The current distribution near the axial plasma column during the explosive decay of the column has been monitored and correlated with the electron beam production. Plasma focus discharges by our mode of operation generate high-intensity

The influence of pulsed electric fields and microwave pretreatments on some selected physicochemical properties of oil extracted from black cumin seed.

PubMed

Bakhshabadi, Hamid; Mirzaei, HabibOllah; Ghodsvali, Alireza; Jafari, Seid Mahdi; Ziaiifar, Aman Mohammad

2018-01-01

Application of novel technologies such as microwave and pulsed electric fields (PEF) might increase the speed and efficiency of oil extraction. In the present research, PEF (3.25 kV/cm electric field intensity and 30 pulse number) and microwave (540 W for 180 s) pretreatments were used to study the process of oil extraction from black cumin ( Nigella sativa ) seeds. After applying the selected pretreatments, the oil of seeds was extracted with the use of a screw press and the extraction efficiency, refractive index, oil density, color index, oxidative stability, and chemical components of oil and protein of meal were evaluated. The achieved results expressed that PEF and microwave pretreatments increased the oil extraction efficiency and its oxidative stability. Different pretreatments didn't have any significant influence on the refractive index of black cumin seed oil ( p >.05). When microwave and PEF were used, the oil density showed an enhancement as the following: 1.51% and 0.96%, respectively in comparison with the samples with no pretreatments. Evaluation of the extracted oils, using GC/MS analysis indicated that thymoquinone was the dominant phenolic component in the black cumin oil. Finally, the SEM analysis revealed that microwave and PEF can be useful in the extraction of oil from black cumin seeds since these treatments damaged cell walls and facilitated the oil extraction process.

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.

Determination of chloramphenicol and zeranols in pig muscle by immunoaffinity column clean-up and LC-MS/MS analysis.

PubMed

Wang, Qing; Zhao, Hua; Xi, Cunxian; Wang, Guomin; Chen, Dongdong; Ding, Shijia

2014-01-01

An immunoaffinity column clean-up and LC-MS/MS method was successfully developed for simultaneous determination of chloramphenicol, zearalanone, α-zearalanol, β-zearalanol, zearalenone, α-zearalenol and β-zearalenol in pig muscle. The sample was extracted with diethyl ether after enzymatic digestion by β-glucuronidase/sulfatase. The extracted solution was evaporated to dryness and the residue was then dissolved in 1 ml of 50% acetonitrile solution. After filtration and dilution with phosphate buffer solution (PBS), the reconstituted solution was cleaned-up with an IAC-CZ immunoaffinity column and then analysed by HPLC-MS/MS. The established method were validated by linearity (r ≥ 0.9990), precision (RSD ≥ 2.9%), average recovery (74.5-105.0%) and limit of detection (0.04-0.10 μg kg(-1)). The developed method is rapid, reliable, sensitive, accurate and has good applicability for real samples.

A PROCESS FOR SEPARATING AZEOTROPIC MIXTURES BY EXTRACTIVE AND CONVECTIVE DISTILLATION

DOEpatents

Frazer, J.W.

1961-12-19

A method is described for separating an azeotrope of carbon tetrachloride and 1,1,2,2-tetrafluorodinitroethane boiling at 60 deg C. The ndethod comnprises, specifically, feeding azeotrope vapors admixed with a non- reactive gas into an extractive distillation column heated to a temperature preferably somewhat above the boiling point of the constant boiling mixture. A solvent, di-n-butylphthalate, is metered into the column above the gas inlet and permitted to flow downward, earrying with it the higher bomling fraction, while the constituent having the lower boiling point passes out of the top of the column with the non-reactive gas and is collected in a nitrogen cold trap. Other solvents which alter the vapor pressure relationship may be substituted. The method is generally applicable to azeotropic mixtures. A number of specific mixtures whicb may be separated are disclosed. (AEC)

CPU and GPU-based Numerical Simulations of Combustion Processes

DTIC Science & Technology

2012-04-27

Distribution unlimited UCLA MAE Research and Technology Review April 27, 2012 Magnetohydrodynamic Augmentation of the Pulse Detonation Rocket Engines...Pulse Detonation Rocket-Induced MHD Ejector (PDRIME) – Energy extract from exhaust flow by MHD generator – Seeded air stream acceleration by MHD...accelerator for thrust enhancement and control • Alternative concept: Magnetic piston – During PDE blowdown process, MHD extracts energy and

Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory; determination of organophosphate pesticides in filtered water by gas chromatography with flame photometric detection

USGS Publications Warehouse

Jha, Virendra K.; Wydoski, Duane S.

2002-01-01

A method for the isolation of 20 parent organophosphate pesticides and 5 pesticide degradates from filtered natural-water samples is described. Seven of these compounds are reported permanently with an estimated concentration because of performance issues. Water samples are filtered to remove suspended particulate matter, and then 1 liter of filtrate is pumped through disposable solid-phase extraction columns that contain octadecyl-bonded porous silica to extract the compounds. The C-18 columns are dried with nitrogen gas, and method compounds are eluted from the columns with ethyl acetate. The extract is analyzed by dual capillary-column gas chromatography with flame photometric detection. Single-operator method detection limits in all three water-matrix samples ranged from 0.004 to 0.012 microgram per liter. Method performance was validated by spiking all compounds into three different matrices at three different concentrations. Eight replicates were analyzed at each concentration level in each matrix. Mean recoveries of method compounds spiked in surface-water samples ranged from 39 to 149 percent and those in ground-water samples ranged from 40 to 124 percent for all pesticides except dimethoate. Mean recoveries of method compounds spiked in reagent-water samples ranged from 41 to 119 percent for all pesticides except dimethoate. Dimethoate exhibited reduced recoveries (mean of 43 percent in low- and medium-concentration level spiked samples and 20 percent in high-concentration level spiked samples) in all matrices because of incomplete collection on the C-18 column. As a result, concen-trations of dimethoate and six other compounds (based on performance issues) in samples are reported in this method with an estimated remark code.

HPLC-MS-MS Determination of ZCZ-011, A Novel Pharmacological Tool for Investigation of the Cannabinoid Receptor in Mouse Brain Using Clean Screen FASt™ Column Extraction.

PubMed

Poklis, Justin L; Clay, Deborah J; Ignatowska-Jankowska, Bogna M; Zanato, Chiara; Ross, Ruth A; Greig, Iain R; Abdullah, Rehab A; Mustafa, Mohammed A; Lichtman, Aron H; Poklis, Alphonse

2015-06-01

A high-performance liquid chromatography tandem mass spectrometry method was developed for the detection and quantification of 6-methyl-3-(2-nitro-1-(thiophen-2-yl)propyl)-2-phenyl-1H-indole (ZCZ-011) using 2-phenylindole as the internal standard (ISTD). ZCZ-011 was synthesized as a possible positive allosteric modulator with the CB1 cannabinoid receptor. The analytical method employs a rapid extraction technique using Clean Screen FASt™ columns with a Positive Pressure Manifold. FASt™ columns were originally developed for urine drug analysis but we have successfully adapted them to the extraction of brain tissue. Chromatographic separation was performed on a Restek Allure Biphenyl 5 µ, 100 × 3.2 mm column (Bellefonte, PA). The mobile phase consisted of 1:9 deionized water with 10 mmol ammonium acetate and 0.1% formic acid-methanol. The following transition ions (m/z) were monitored for ZCZ-011: 363 > 207 and 363 > 110 and for the ISTD: 194 > 165 and 194 > 89. The FASt™ columns lowered and stabilized the ion suppression over the linear range of the assay (40-4,000 ng/g). The method was evaluated for recovery, ion suppression, accuracy/bias, intraday and interday precision, bench-top stability, freeze-thaw and post-preparative stability. The method was successfully applied to brain tissue from C57BL/6J mice that received intraperitoneal (i.p.) injections with 40 mg/kg of ZCZ-011 or vehicle. © The Author 2015. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Effect of chemical and physical heterogeneities on colloid-facilitated cesium transport

NASA Astrophysics Data System (ADS)

Rod, Kenton; Um, Wooyong; Chun, Jaehun; Wu, Ning; Yin, Xialong; Wang, Guohui; Neeves, Keith

2018-06-01

A set of column experiments was conducted to investigate the chemical and physical heterogeneity effect on colloid facilitated transport under slow pore velocity conditions. Pore velocities were kept below 100 cm d-1 for all experiments. Glass beads were packed into columns establishing four different conditions: 1) homogeneous, 2) mixed physical heterogeneity, 3) sequentially layered physical heterogeneity, and 4) chemical heterogeneity. The homogeneous column was packed with glass beads (diameter 500-600 μm), and physical heterogeneities were created by sequential layering or mixing two sizes of glass bead (500-600 μm and 300-400 μm). A chemical heterogeneity was created using 25% of the glass beads coated with hydrophobic molecules (1H-1H-2H-2H-perfluorooctyltrichlorosilane) mixed with 75% pristine glass beads (all 500-600 μm). Input solution with 0.5 mM CsI and 50 mg L-1 colloids (1-μm diameter SiO2) was pulsed into columns under saturated conditions. The physical heterogeneity in the packed glass beads retarded the transport of colloids compared to homogeneous (R = 25.0), but showed only slight differences between sequentially layered (R = 60.7) and mixed heterogeneity(R = 62.4). The column with the chemical, hydrophobic/hydrophilic, heterogeneity removed most of the colloids from the input solution. All column conditions stripped Cs from colloids onto the column matrix of packed glass beads.

Enhancement of SPES source performances.

PubMed

Fagotti, E; Palmieri, A; Ren, X

2008-02-01

Installation of SPES source at LNL was finished in July 2006 and the first beam was extracted in September 2006. Commissioning results confirmed very good performance of the extracted current density. Conversely, source reliability was very poor due to glow-discharge phenomena, which were caused by the ion source axial magnetic field protruding in the high-voltage column. This problem was fixed by changing the stainless steel plasma electrode support with a ferromagnetic one. This new configuration required us to recalculate ion source solenoids positions and fields in order to recover the correct resonance pattern. Details on magnetic simulations and experimental results of high voltage column shielding are presented.

Insecticidal effect of plant extracts on Phlebotomus argentipes (Diptera: Psychodidae) in Bihar, India.

PubMed

Dinesh, Diwakar Singh; Kumari, Seema; Pandit, Vibhishan; Kumar, Jainendra; Kumari, Nisha; Kumar, Prahlad; Hassan, Faizan; Kumar, Vijay; Das, Pradeep

2015-12-01

Phlebotomus argentipes (Diptera: Psychodidae), the established vector for kala-azar is presently being controlled by indoor residual spray of DDT in kala-azar endemic areas in India. Search for non-hazardous and non-toxic biodegradable active molecules from botanicals may provide cost-effective and eco-friendly alternatives to synthetic insecticides. The present study was aimed at evaluating various plant extracts from endemic and non-endemic areas of Bihar for their insecticidal activity against sandfly to identify the most effective plant extract. Bio-assay test was conducted with larvae and adult of P. argentipes with different plant extracts collected in distilled water, hexane, ethyl acetate, acetone and methanol. Thin layer chromatography (TLC), column chromatography and high performance liquid chromatography (HPLC) were conducted for detection of active molecules. Adults and larvae of sandflies exposed to the aqueous extract of Nicotiana tabacum resulted in 100 per cent mortality. The hexane extract of Clerodendrum infortunatum was found to kill 77 per cent adults but was ineffective against larvae. Bio-assay test of the ninth fraction (hexane extract-methanol phase) separated by column chromatography was found to be 63 per cent effective. The purple spot on the TLC of this fraction indicated the presence of a diterpenoid. HPLC of this fraction detected nine compounds with two peaks covering 20.44 and 56.52 per cent areas with retention time of 2.439 and 5.182 min, respectively supporting the TLC results. The column separated 9 [th] fraction of C. infortunatum extract was found to be effective in killing 63 per cent of adult P. argentipes. Compounds of this fraction need to be evaluated further for identification and characterization of the active molecule by conducting individual bio-assay tests followed by further fractionation and HPLC. Once the structure of the active molecule is identified and validated, it may be synthesized and formulated as a product.

Efficient purification of paclitaxel from yews using high-performance displacement chromatography technique.

PubMed

Watchueng, Jean; Kamnaing, Pierre; Gao, Jin-Ming; Kiyota, Taira; Yeboah, Faustinus; Konishi, Yasuo

2011-05-20

Paclitaxel was purified using high-performance displacement chromatography (HPDC) technique, but not by the mechanism of HPDC. On small scale, paclitaxel was extracted with methanol from dry needles of Taxus canadensis and was enriched by extracting with chloroform after removing water-soluble hydrophilic components and hexane-soluble hydrophobic components. Then, 93-99% purity of paclitaxel was obtained using the HPDC technique. On large scale, taxanes were enriched by solvent partitioning between acetic acid/MeOH/H(2)O and hexane and extracted with CH(2)Cl(2). Taxanes except paclitaxel were further removed by extracting with methanol-water-trifluoroacetic acid (1.0:98.9:0.1, v/v/v). Applying HPDC technique to water-insoluble substances is problematic as this method requires a highly aqueous solvent system. In order to overcome this incompatibility, a system was set up where paclitaxel, although in low concentration, was extracted by methanol-water-trifluoroacetic acid (10.0:89.9:0.1, v/v/v). Recycling the extracting solvent to ensure minimal volume, the extracted paclitaxel was adsorbed on a C(18) trap column. A C(18) column of 4.6mm internal diameter was then connected to the trap column. The HPDC technique was thus carried out using an isocratic acetonitrile-water-trifluoroacetic acid (30.0:69.9:0.1, v/v/v) mobile phase consisting of a displacer cetylpyridinium trifluoroacetate (3mg/mL). Paclitaxel was co-eluted with the displacer and spontaneously crystallized. The crystal (114mg) showed 99.4% purity and only 10% of paclitaxel in the starting crude extract was lost during the enrichment/purification processes. This large scale purification method was successfully applied to purify paclitaxel from Chinese yew in small scale, suggesting general applicability of the method. This is the first report of purifying a water-insoluble natural product using HPDC technique. Crown Copyright © 2011. Published by Elsevier B.V. All rights reserved.

Insecticidal effect of plant extracts on Phlebotomus argentipes (Diptera: Psychodidae) in Bihar, India

PubMed Central

Dinesh, Diwakar Singh; Kumari, Seema; Pandit, Vibhishan; Kumar, Jainendra; Kumari, Nisha; Kumar, Prahlad; Hassan, Faizan; Kumar, Vijay; Das, Pradeep

2015-01-01

Background & objectives: Phlebotomus argentipes (Diptera: Psychodidae), the established vector for kala-azar is presently being controlled by indoor residual spray of DDT in kala-azar endemic areas in India. Search for non-hazardous and non-toxic biodegradable active molecules from botanicals may provide cost-effective and eco-friendly alternatives to synthetic insecticides. The present study was aimed at evaluating various plant extracts from endemic and non-endemic areas of Bihar for their insecticidal activity against sandfly to identify the most effective plant extract. Methods: Bio-assay test was conducted with larvae and adult of P. argentipes with different plant extracts collected in distilled water, hexane, ethyl acetate, acetone and methanol. Thin layer chromatography (TLC), column chromatography and high performance liquid chromatography (HPLC) were conducted for detection of active molecules. Results: Adults and larvae of sandflies exposed to the aqueous extract of Nicotiana tabacum resulted in 100 per cent mortality. The hexane extract of Clerodendrum infortunatum was found to kill 77 per cent adults but was ineffective against larvae. Bio-assay test of the ninth fraction (hexane extract-methanol phase) separated by column chromatography was found to be 63 per cent effective. The purple spot on the TLC of this fraction indicated the presence of a diterpenoid. HPLC of this fraction detected nine compounds with two peaks covering 20.44 and 56.52 per cent areas with retention time of 2.439 and 5.182 min, respectively supporting the TLC results. Interpretation & conclusions: The column separated 9th fraction of C. infortunatum extract was found to be effective in killing 63 per cent of adult P. argentipes. Compounds of this fraction need to be evaluated further for identification and characterization of the active molecule by conducting individual bio-assay tests followed by further fractionation and HPLC. Once the structure of the active molecule is identified and validated, it may be synthesized and formulated as a product. PMID:26905249

Quantitative analysis of three chiral pesticide enantiomers by high-performance column liquid chromatography.

PubMed

Wang, Peng; Liu, Donghui; Gu, Xu; Jiang, Shuren; Zhou, Zhiqiang

2008-01-01

Methods for the enantiomeric quantitative determination of 3 chiral pesticides, paclobutrazol, myclobutanil, and uniconazole, and their residues in soil and water are reported. An effective chiral high-performance liquid chromatographic (HPLC)-UV method using an amylose-tris(3,5-dimethylphenylcarbamate; AD) column was developed for resolving the enantiomers and quantitative determination. The enantiomers were identified by a circular dichroism detector. Validation involved complete resolution of each of the 2 enantiomers, plus determination of linearity, precision, and limit of detection (LOD). The pesticide enantiomers were isolated by solvent extraction from soil and C18 solid-phase extraction from water. The 2 enantiomers of the 3 pesticides could be completely separated on the AD column using n-hexane isopropanol mobile phase. The linearity and precision results indicated that the method was reliable for the quantitative analysis of the enantiomers. LODs were 0.025, 0.05, and 0.05 mg/kg for each enantiomer of paclobutrazol, myclobutanil, and uniconazole, respectively. Recovery and precision data showed that the pretreatment procedures were satisfactory for enantiomer extraction and cleanup. This method can be used for optical purity determination of technical material and analysis of environmental residues.

Simultaneous column chromatographic extraction and purification of abscisic acid in peanut plants for direct HPLC analysis.

PubMed

Zhang, Ya-Wen; Fan, Wei-Wei; Li, Hui; Ni, He; Han, Han-Bing; Li, Hai-Hang

2015-10-01

Abscisic acid (ABA), a universal signaling molecule, plays important roles in regulating plant growth, development and stress responses. The low contents and complex components in plants make it difficult to be accurately analyzed. A novel one-step sample preparation method for ABA in plants was developed. Fresh peanut (Arachis hypogaea) plant materials were fixed by oven-drying, microwave drying, boiling or Carnoy's fixative, and loaded onto a mini-preparing column. After washed the impurities, ABA was eluted with a small amount of solvent. ABA in plant materials was completely extracted and purified in 2mL solution and directly analyzed by HPLC, with a 99.3% recovery rate. Multiple samples can be simultaneously prepared. Analyses using this method indicated that the endogenous ABA in oven-dried peanut leaves increased 20.2-fold from 1.01 to 20.37μgg(-1) dry weight within 12h and then decreased in 30% polyethylene glycol 6000 treated plants, and increased 3.34-fold from 0.85 to 2.84μgg(-1) dry weight in 5 days and then decreased in soil drought treated plants. The method combined the column chromatographic extraction and solid-phase separation technologies in one step and can completely extracted plant endogenous ABA in a purified and highly concentrated form for direct HPLC analysis. Copyright © 2015 Elsevier B.V. All rights reserved.

Immunochromatographic assay of cadmium levels in oysters.

PubMed

Nishi, Kosuke; Kim, In-Hae; Itai, Takaaki; Sugahara, Takuya; Takeyama, Haruko; Ohkawa, Hideo

2012-08-15

Oysters are one of foodstuffs containing a relatively high amount of cadmium. Here we report on establishment of an immunochromatographic assay (ICA) method of cadmium levels in oysters. Cadmium was extracted with 0.l mol L(-1) HCl from oysters and cleaned up from other metals by the use of an anion-exchange column. The behavior of five metals Mn, Fe, Cu, Zn, and Cd was monitored at each step of extraction and clean-up procedure for the ICA method in an inductively coupled plasma-mass spectrometry (ICP-MS) analysis. The results revealed that a simple extraction method with the HCl solution was efficient enough to extract almost all of cadmium from oysters. Clean-up with an anion-exchange column presented almost no loss of cadmium adsorbed on the column and an efficient removal of metals other than cadmium. When a spiked recovery test was performed in the ICA method, the recovery ranged from 98% to 112% with relative standard deviations between 5.9% and 9.2%. The measured values of cadmium in various oyster samples in the ICA method were favorably correlated with those in ICP-MS analysis (r(2)=0.97). Overall results indicate that the ICA method established in the present study is an adequate and reliable detection method for cadmium levels in oysters. Copyright © 2012 Elsevier B.V. All rights reserved.

Double-shot MeV electron diffraction and microscopy

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

Musumeci, P.; Cesar, D.; Maxson, J.

Here in this paper, we study by numerical simulations a time-resolved MeV electron scattering mode where two consecutive electron pulses are used to capture the evolution of a material sample on 10 ps time scales. The two electron pulses are generated by illuminating a photocathode in a radiofrequency photogun by two short laser pulses with adjustable delay. A streak camera/deflecting cavity is used after the sample to project the two electron bunches on two well separated regions of the detector screen. By using sufficiently short pulses, the 2D spatial information from each snapshot can be preserved. This “double-shot” technique enablesmore » the efficient capture of irreversible dynamics in both diffraction and imaging modes. Finally, in this work, we demonstrate both modes in start-to-end simulations of the UCLA Pegasus MeV microscope column.« less

Double-shot MeV electron diffraction and microscopy

DOE PAGES

Musumeci, P.; Cesar, D.; Maxson, J.

2017-05-19

Here in this paper, we study by numerical simulations a time-resolved MeV electron scattering mode where two consecutive electron pulses are used to capture the evolution of a material sample on 10 ps time scales. The two electron pulses are generated by illuminating a photocathode in a radiofrequency photogun by two short laser pulses with adjustable delay. A streak camera/deflecting cavity is used after the sample to project the two electron bunches on two well separated regions of the detector screen. By using sufficiently short pulses, the 2D spatial information from each snapshot can be preserved. This “double-shot” technique enablesmore » the efficient capture of irreversible dynamics in both diffraction and imaging modes. Finally, in this work, we demonstrate both modes in start-to-end simulations of the UCLA Pegasus MeV microscope column.« less

Development of an Airborne Triple-Pulse 2-Micron Integrated Path Differential Absorption Lidar (IPDA) for Simultaneous Airborne Column Measurements of Carbon Dioxide and Water Vapor in the Atmosphere

NASA Technical Reports Server (NTRS)

Singh, Upendra N.; Petros, Mulugeta; Refaat, Tamer F.; Yu, Jirong; Antill, Charles W.; Remus, Ruben

2016-01-01

This presentation will provide status and details of an airborne 2-micron triple-pulse integrated path differential absorption (IPDA) lidar being developed at NASA Langley Research Center with support from NASA ESTO Instrument Incubator Program. The development of this active optical remote sensing IPDA instrument is targeted for measuring both atmospheric carbon dioxide and water vapor in the atmosphere from an airborne platform. This presentation will focus on the advancement of the 2-micron triple-pulse IPDA lidar development. Updates on the state-of-the-art triple-pulse laser transmitter will be presented including the status of seed laser locking, wavelength control, receiver and detector upgrades, laser packaging and lidar integration. Future plan for IPDA lidar system for ground integration, testing and flight validation will also be presented.

Monolithic silica spin column extraction and simultaneous derivatization of amphetamines and 3,4-methylenedioxyamphetamines in human urine for gas chromatographic-mass spectrometric detection.

PubMed

Nakamoto, Akihiro; Nishida, Manami; Saito, Takeshi; Kishiyama, Izumi; Miyazaki, Shota; Murakami, Katsunori; Nagao, Masataka; Namura, Akira

2010-02-19

A simple, sensitive, and specific method with gas chromatography-mass spectrometry was developed for simultaneous extraction and derivatization of amphetamines (APs) and 3,4-methylenedioxyamphetamines (MDAs) in human urine by using a monolithic silica spin column. All the procedures, such as sample loading, washing, and elution were performed by centrifugation. APs and MDAs in urine were adsorbed on the monolithic silica and derivatized with propyl chloroformate in the column. Methamphetamine-d(5) was used as an internal standard. The linear ranges were 0.01-5.0 microg mL(-1) for methamphetamine (MA) and 3,4-methylenedioxymethamphetamine (MDMA) and 0.02-5.0 microg mL(-1) for amphetamine (AP) and 3,4-methylenedioxyamphetamine (MDA) (coefficient of correlation > or = 0.995). The recovery of APs and MDAs in urine was 84-94%, and the relative standard deviation of the intra- and interday reproducibility for urine samples containing 0.1, 1.0, and 4.0 microg mL(-1) of APs and MDAs ranged from 1.4% to 13.6%. The lowest detection limit (signal-to-noise ratio > or = 3) in urine was 5 ng mL(-1) for MA and MDMA and 10 ng mL(-1) for AP and MDA. The proposed method can be used to perform simultaneous extraction and derivatization on spin columns that have been loaded with a small quantity of solvent by using centrifugation. Copyright 2009 Elsevier B.V. All rights reserved.

Graphene oxide-based composite monolith as new sorbent for the on-line solid phase extraction and high performance liquid chromatography determination of ß-sitosterol in food samples.

PubMed

Cui, Beijiao; Guo, Bin; Wang, Huimin; Zhang, Doudou; Liu, Haiyan; Bai, Ligai; Yan, Hongyuan; Han, Dandan

2018-08-15

A composite monolithic column was prepared by redox initiation method for the on-line purification and enrichment of β-sitosterol, in which graphene oxide (GO) was embedded. The obtained monolithic column was characterized by scanning electron microscopy (SEM) and nitrogen adsorption-desorption isotherm measurement, which indicated that the monolith possessed characteristics of porous structure and high permeability. Under the optimum conditions for extraction and determination, the calibration equation was y = 47.92 × -0.1391; the linear range was 0.008-1.0 mg mL -1 ; the linear regression coefficient was 0.998; the limit of detection (LOD) is 2.4 μg mL -1 ; the limit of quantitation (LOQ) was 8 μg mL -1 ; precisions for intra-day and inter-day assays presented as relative standard deviations were less than 4.3% and 6.8%, respectively. Under the selective conditions, the enrichment factor of the method was 119. The recovery was in the range of 80.40-98.00%. Moreover, the adsorption amount of the monolith was compared with silica gel-C18 adsorbent and the monolith without graphene oxide being embedded. The polymerization monolithic column showed high selectivity and good permeability, and it was successfully used as on-line solid-phase extraction (SPE) column for determination of β-sitosterol in edible oil. Copyright © 2018 Elsevier B.V. All rights reserved.

Methods of analysis by the U.S. Geological Survey Organic Geochemistry Research Group : determination of selected herbicides and their degradation products in water using solid-phase extraction and gas chromatography/mass spectrometry

USGS Publications Warehouse

Kish, J.L.; Thurman, E.M.; Scribner, E.A.; Zimmerman, L.R.

2000-01-01

A method for the extraction and analysis of eight herbicides and five degradation products using solid-phase extraction from natural water samples followed by gas chromatography/mass spectrometry is presented in this report. This method was developed for dimethenamid; flufenacet; fluometuron and its degradation products, demethylfluometuron (DMFM), 3-(trifluromethyl)phenylurea (TFMPU), 3-(trifluromethyl)-aniline (TFMA); molinate; norflurazon and its degradation product, demethylnorflurazon; pendamethalin; the degradation product of prometryn, deisopropylprometryn; propanil; and trifluralin. The eight herbicides are used primarily in the southern United States where cotton, rice, and soybeans are produced. The exceptions are dimethenamid and flufenacet, which are used on corn in the Midwest. Water samples received by the U.S. Geological Survey's Organic Geochemistry Research Group in Lawrence, Kansas, are filtered to remove suspended particulate matter and then passed through disposable solid-phase extraction columns containing octadecyl-bonded porous silica (C-18) to extract the compounds. The herbicides and their degradation products are removed from the column by ethyl acetate elution. The eluate is evaporated under nitrogen, and components then are separated, identified, and quantified by injecting an aliquot of the concentrated extract into a high-resolution, fused-silica capillary column of a gas chromatograph/mass spectrometer under selected-ion mode. Method detection limits ranged from 0.02 to 0.05 ?g/L for all compounds with the exception of TFMPU, which has a method detection limit of 0.32 ?g/L. The mean absolute recovery is 107 percent. This method for the determination of herbicides and their degradation products is valuable for acquiring information about water quality and compound fate and transport in water.

Application of an online post-column derivatization HPLC-DPPH assay to detect compounds responsible for antioxidant activity in Sonchus oleraceus L. leaf extracts.

PubMed

Ou, Zong-Quan; Schmierer, David M; Rades, Thomas; Larsen, Lesley; McDowell, Arlene

2013-02-01

To use an online assay to identify key antioxidants in Sonchus oleraceus leaf extracts and to investigate the effect of leaf position and extraction conditions on antioxidant concentration and activity. Separation of phytochemicals and simultaneous assessment of antioxidant activity were performed online using HPLC and post-column reaction with a free-radical reagent (2, 2-diphenylpicrylhydrazyl, DPPH). Active compounds were identified using nuclear magnetic resonance spectroscopy and mass spectrometry. We applied the online HPLC-DPPH radical assay to evaluate antioxidants in leaves from different positions on the plant and to assess the effect of pre-treatment of leaves with liquid N(2) before grinding, extraction time, extraction temperature and method of concentrating extracts. Key antioxidants identified in S. oleraceus leaf extracts were caftaric acid, chlorogenic acid and chicoric acid. Middle leaves contained the highest total amount of the three key antioxidant compounds, consisting mainly of chicoric acid. Pre-treatment with liquid N(2), increasing the extraction temperature and time and freeze-drying the extract did not enhance the yield of the key antioxidants. The online HPLC-DPPH radical assay was validated as a useful screening tool for investigating individual antioxidants in leaf extracts. Optimized extraction conditions were middle leaves pre-treated with liquid N(2), extraction at 25°C for 0.5 h and solvent removal by rotary evaporation. © 2012 The Authors. JPP © 2012. Royal Pharmaceutical Society.

Development of the front end test stand and vessel for extraction and source plasma analyses negative hydrogen ion sources at the Rutherford Appleton Laboratory.

PubMed

Lawrie, S R; Faircloth, D C; Letchford, A P; Perkins, M; Whitehead, M O; Wood, T; Gabor, C; Back, J

2014-02-01

The ISIS pulsed spallation neutron and muon facility at the Rutherford Appleton Laboratory (RAL) in the UK uses a Penning surface plasma negative hydrogen ion source. Upgrade options for the ISIS accelerator system demand a higher current, lower emittance beam with longer pulse lengths from the injector. The Front End Test Stand is being constructed at RAL to meet the upgrade requirements using a modified ISIS ion source. A new 10% duty cycle 25 kV pulsed extraction power supply has been commissioned and the first meter of 3 MeV radio frequency quadrupole has been delivered. Simultaneously, a Vessel for Extraction and Source Plasma Analyses is under construction in a new laboratory at RAL. The detailed measurements of the plasma and extracted beam characteristics will allow a radical overhaul of the transport optics, potentially yielding a simpler source configuration with greater output and lifetime.

Sensitive method for the quantitation of droloxifene in plasma and serum by high-performance liquid chromatography employing fluorimetric detection.

PubMed

Tess, D A; Cole, R O; Toler, S M

1995-12-15

A simple and highly sensitive reversed-phase fluorimetric HPLC method for the quantitation of droloxifene from rat, monkey, and human plasma as well as human serum is described. This assay employs solid-phase extraction and has a dynamic range of 25 to 10,000 pg/ml. Sample extraction (efficiencies > 86%) was accomplished using a benzenesulfonic acid (SCX) column with water and methanol rinses. Droloxifene and internal standard were eluted with 1 ml of 3.5% (v/v) ammonium hydroxide (30%) in methanol. Samples were quantitated using post-column UV-photochemical cyclization coupled with fluorimetric detection with excitation and emission wavelengths of 260 nm and 375 nm, respectively. Relative ease of sample extraction and short run times allow for the analysis of approximately 100 samples per day.

Comparison of methods for hydrocarbon analysis of marine biota

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

Gritz, R.L.; Shaw, D.G.

1977-04-01

A comparison was made of several procedures for the isolation of hydrocarbons from other matter and for the fractionation of hydrocarbons according to chemical type. The efficiency of Soxhlet extraction followed by saponification with extraction by alkaline digestion (direct saponification) was compared using two hour and 24 hour reaction times. All procedures were performed on approximately 60 g of soft parts of Saxidomus gigantea (butter clam). The 24 hour saponification and column chromatography on partially deactivated columns constituted the best procedure tested. Soxhlet extraction followed by two hour saponification did not completely remove methyl esters and was the most laboriousmore » technique. Direct two hour saponification was also questionable in the removal of esters and led to severe emulsion problems. The recoveries of hydrocarbons by the three procedures was substantially the same.« less

Characterization of the molluscicidal activity of Bauhinia variegata and Mimusops elengi plant extracts against the fasciola vector Lymnaea acuminata.

PubMed

Singh, Kanchan Lata; Singh, D K; Singh, Vinay Kumar

2012-01-01

The molluscicidal activity of Bauhinia variegata leaf and Mimusops elengi bark was studied against vector snail Lymnaea acuminata. The toxicity of both plants was time and concentration-dependent. Among organic extracts, ethanol extracts of both plants were more toxic. Toxicity of B. variegata leaf ethanolic extract (96h LC50- 14.4 mg/L) was more pronounced than M. elengi bark ethanolic extract (96h LC50-15.0 mg/L). The 24h LC50 of column purified fraction of B. variegata and M. elengi bark were 20.3 mg/L and 18.3 mg/L, respectively. Saponin and quercetin were characterized and identified as active molluscicidal component. Co-migration of saponin (Rf 0.48) and quercetin (Rf 0.52) with column purified bark of M. elengi and leaf of B. variegata on thin layer chromatography demonstrate same Rf value i.e. 0.48 and 0.52, respectively. The present study clearly indicates the possibility of using M. elengi and/or B. variegata as potent molluscicide.

Mathematical modeling of the adsorption/desorption characteristics of anthocyanins from muscadine (Vitis rotundifolia cv. Noble) juice pomace on Amberlite FPX66 resin in a fixed bed column.

PubMed

Uzdevenes, Chad G; Gao, Chi; Sandhu, Amandeep K; Yagiz, Yavuz; Gu, Liwei

2018-03-24

Muscadine grape pomace, a by-product of juicing and wine-making, contains significant amounts of anthocyanin 3,5-diglucosides, known to be beneficial to human health. The objective of this research was to use mathematical modeling to investigate the adsorption/desorption characteristics of these anthocyanins from muscadine grape pomace on Amberlite FPX66 resin in a fixed bed column. Anthocyanins were extracted using hot water and ultrasound, and the extracts were loaded onto a resin column at five bed depths (5, 6, 8, 10 and 12 cm) using three flow rates (4, 6 and 8 mL min -1 ). It was found that adsorption on the column fitted the bed depth service time (BDST) model and the empty bed residence time (EBRT) model. Desorption was achieved by eluting the column using ethanol at four concentrations (25, 40, 55 and 70% v/v) and could be described with an empirical sigmoid model. The breakthrough curves of anthocyanins fitted the BDST model for all three flow rates with R 2 values of 0.983, 0.992 and 0.984 respectively. The EBRT model was successfully employed to find the operating lines, which allow for column scale-up while still achieving similar results to those found in a laboratory operation. Desorption with 40% (v/v) ethanol achieved the highest recovery rate of anthocyanins at 79.6%. The mathematical models established in this study can be used in designing a pilot/industrial- scale column for the separation and concentration of anthocyanins from muscadine juice pomace. © 2018 Society of Chemical Industry. © 2018 Society of Chemical Industry.

A new solid-phase extraction and HPLC method for determination of patulin in apple products and hawthorn juice in China.

PubMed

Zhou, Yuchun; Kong, Weijun; Li, Yan; Logrieco, Antonio F; Xu, Jun; Yang, Meihua

2012-03-01

A new solid-phase extraction (SPE) pretreatment method using a home-made polyvinylpolypyrrolidone-florisil (PVPP-F) column was developed for the analysis of patulin in apple and hawthorn products in China. Fifty samples (25 apple juices, 12 apple jams, and 13 hawthorn juices) were prepared using the new method and then analyzed by high performance liquid chromatography with diode array detection (HPLC-DAD) on an Agela Venusil MP C(18) reversed-phase column (4.6 mm × 250 mm, 5 μm). The cleanup results for all samples using home-made PVPP-F column were compared with those obtained using a MycoSep®228 AflaPat column. The correlation coefficient R (0.9998) fulfilled the requirement of linearity for patulin in the concentration range of 2.5-250 μg/kg. The limits of detection (LODs) and quantification (LOQs) of patulin were 3.99 and 9.64 μg/kg for PVPP-F column, and 3.56 and 8.07 μg/kg for MycoSep®228 AflaPat column, respectively. Samples were spiked with patulin at levels ranging from 25 to 250 μg/kg, and recoveries using PVPP-F and MycoSep®228 AflaPat columns were in the range of 81.9-100.9% and 86.4-103.9%, respectively. Naturally occurring patulin was found in 2 of 25 apple juice samples (8.0%) and 1 of 13 hawthorn juice samples (7.7%) at concentrations ranging from 12.26 to 36.81 μg/kg. The positive results were further confirmed by liquid chromatography electrospray ionization mass spectrometry (LC-ESI-MS). © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

An autoregressive model-based particle filtering algorithms for extraction of respiratory rates as high as 90 breaths per minute from pulse oximeter.

PubMed

Lee, Jinseok; Chon, Ki H

2010-09-01

We present particle filtering (PF) algorithms for an accurate respiratory rate extraction from pulse oximeter recordings over a broad range: 12-90 breaths/min. These methods are based on an autoregressive (AR) model, where the aim is to find the pole angle with the highest magnitude as it corresponds to the respiratory rate. However, when SNR is low, the pole angle with the highest magnitude may not always lead to accurate estimation of the respiratory rate. To circumvent this limitation, we propose a probabilistic approach, using a sequential Monte Carlo method, named PF, which is combined with the optimal parameter search (OPS) criterion for an accurate AR model-based respiratory rate extraction. The PF technique has been widely adopted in many tracking applications, especially for nonlinear and/or non-Gaussian problems. We examine the performances of five different likelihood functions of the PF algorithm: the strongest neighbor, nearest neighbor (NN), weighted nearest neighbor (WNN), probability data association (PDA), and weighted probability data association (WPDA). The performance of these five combined OPS-PF algorithms was measured against a solely OPS-based AR algorithm for respiratory rate extraction from pulse oximeter recordings. The pulse oximeter data were collected from 33 healthy subjects with breathing rates ranging from 12 to 90 breaths/ min. It was found that significant improvement in accuracy can be achieved by employing particle filters, and that the combined OPS-PF employing either the NN or WNN likelihood function achieved the best results for all respiratory rates considered in this paper. The main advantage of the combined OPS-PF with either the NN or WNN likelihood function is that for the first time, respiratory rates as high as 90 breaths/min can be accurately extracted from pulse oximeter recordings.

Isolated Attosecond Pulse Generation without the Need to Stabilize the Carrier-Envelope Phase of Driving Lasers

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

Gilbertson, Steve; Khan, Sabih D.; Wu Yi

2010-08-27

Single isolated attosecond pulses can be extracted from a pulse train with an ultrafast gate in the generation target. By setting the gate width sufficiently narrow with the generalized double optical gating, we demonstrate that single isolated attosecond pulses can be generated with any arbitrary carrier-envelope phase value of the driving laser. The carrier-envelope phase only affects the photon flux, not the pulse duration or contrast. Our results show that isolated attosecond pulses can be generated using carrier-envelope phase unstabilized 23 fs pulses directly from chirped pulse amplifiers.

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

Shlapakovski, A.; Gorev, S.; Krasik, Ya. E.

The influence of laser beam parameters on the output pulses of a resonant microwave compressor with a laser-triggered plasma switch was investigated. The S-band compressor, consisting of a rectangular waveguide-based cavity and H-plane waveguide tee with a shorted side arm, was filled with pressurized dry air and pumped by 1.8-μs-long microwave pulses of up to 450 kW power. A Nd:YAG laser was used to ignite the gas discharge in the tee side arm for output pulse extraction. The laser beam (at 213 nm or 532 nm) was directed along the RF electric field lines. It was found that the compressor operated most effectivelymore » when the laser beam was focused at the center of the switch waveguide cross-section. In this case, the power extraction efficiency reached ∼47% at an output power of ∼14 MW, while when the laser beam was not focused the maximal extraction efficiency was only ∼20% at ∼6 MW output power. Focusing the laser beam resulted also in a dramatic decrease (down to <1 ns) in the delay of the output pulses' appearance with respect to the time of the beam's entrance into the switch, and the jitter of the output pulses' appearance was minimized. In addition, the quality of the output pulses' waveform was significantly improved.« less

Automated mini-column solid-phase extraction cleanup for high-throughput analysis of chemical contaminants in foods by low-pressure gas chromatography – tandem mass spectrometry

USDA-ARS?s Scientific Manuscript database

This study demonstrated the application of an automated high-throughput mini-cartridge solid-phase extraction (mini-SPE) cleanup for the rapid low-pressure gas chromatography – tandem mass spectrometry (LPGC-MS/MS) analysis of pesticides and environmental contaminants in QuEChERS extracts of foods. ...

OPTIMIZED DETERMINATION OF TRACE JET FUEL VOLATILE ORGANIC COMPOUNDS IN HUMAN BLOOD USING IN-FIELD LIQUID-LIQUID EXTRACTION WITH SUBSEQUENT LABORATORY GAS CHROMATOGRAPHIC-MASS SPECTROMETRIC ANALYSIS AND ON-COLUMN LARGE VOLUME INJECTION

EPA Science Inventory

A practical and sensitive method to assess volatile organic compounds (VOCs) from JP-8 jet fuel in human whole blood was developed by modifying previously established liquid-liquid extraction procedures, optimizing extraction times, solvent volume, specific sample processing te...

[Simultaneous determination of 15 industrial synthetic dyes in condiment by solid phase extraction-high performance liquid chromatography].

PubMed

Liu, Min; Li, Xiaolin; Bie, Wei; Wang, Minglin; Feng, Qian

2011-02-01

A new method was established for the determination of 15 industrial synthetic dyes in condiment by solid phase extraction-high performance liquid chromatography (SPE-HPLC). The samples were extracted by methanol-water (1:1, v/v) and purified by a solid phase extraction column. Then, the chromatographic separation was achieved on a Luna C18 column by linear gradient elution. The mobile phase was 10 mmol/L ammonium acetate-acetonitrile (containing 1% acetic acid). The results showed that the 15 industrial synthetic dyes can be separated efficiently. The recoveries of the 15 industrial synthetic dyes spiked in condiment were between 84.6% and 114.2% with the relative standard deviations of 0.9% - 10.3%. The limits of detection of this method was 0.05 - 0.18 mg/kg for the 15 industrial synthetic dyes. The method is simple, sensitive, accurate, repeatable and can be used for simultaneous determination of the 15 illegally added industrial synthetic dyes.

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

Molecularly imprinted solid-phase extraction sorbent for the clean-up of chlorinated phenoxyacids from aqueous samples.

PubMed

Baggiani, C; Giovannoli, C; Anfossi, L; Tozzi, C

2001-12-14

A molecularly imprinted polymer (MIP) was synthesized using the herbicide 2,4,5-trichlorophenoxyacetic acid as a template, 4-vinylpyridine as an interacting monomer, ethylendimethacrylate as a cross-linker and a methanol-water mixture as a porogen. The binding properties and the selectivity of the polymer towards the template were investigated by frontal and zonal liquid chromatography. The polymer was used as a solid-phase extraction material for the clean-up of the template molecule and some related herbicides (2,4-dichlorophenoxyacetic acid, fenoprop, dichlorprop) from river water samples at a concentration level of ng/ml with quantitative recoveries comparable with those obtained with a traditional C18 reversed-phase column when analyzed by capillary electrophoresis. The results obtained show that the MIP-based approach to the solid-phase extraction is comparable with the more traditional solid-phase extraction with C18 reversed-phase columns in terms of recovery, but it is superior in terms of sample clean-up.

Fingerprint chromatogram analysis of extracts from the leaves of Tripterygium wilfordii Hook. F. by high performance liquid chromatography.

PubMed

Li, Ke; Wang, Shudong

2005-05-01

A simple and reliable high performance liquid chromatographic (HPLC) method has been developed and validated for the study of fingerprint chromatograms of extracts from the leaves of Tripterygium wilfordii Hook. F. (TWHF) and for controlling the quality of the herb. HPLC separation of the extracts was performed on a Lichrospher RP-18 column and detected by ultraviolet absorbance at 210 nm. The column temperature was maintained at 35 degrees C. A mobile phase composed of acetonitrile:H2O in the ratio of 39:61 (v/v) was found to be most suitable for this separation at a flow rate of 0.8 mL/min with isocratic elution. Under the chromatographic conditions described, the peak profile of the 10 components collected within 35 min made up the fingerprint of the extracts from leaves of TWHF with universal features. The fingerprint chromatograms had a good stability, precision, and reproducibility. The similarity of the extracts from leaves of TWHF collected in summer and winter was studied with triptolide as a reference peak. The method is suitable for differentiation of extracts from the leaves of TWHF, and can be used as a quality control method for this herb.

Cytotoxic and multidrug resistance reversal activity of a vegetable, 'Anastasia Red', a variety of sweet pepper.

PubMed

Motohashi, Noboru; Wakabayashi, Hidetsugu; Kurihara, Teruo; Takada, Yuko; Maruyama, Shichiro; Sakagami, Hiroshi; Nakashima, Hideki; Tani, Satoru; Shirataki, Yoshiaki; Kawase, Masami; Wolfard, Kristina; Molnár, Joseph

2003-04-01

The vegetable, Anastasia Red, Capsicum annuum L. var. angulosum Mill. (Solanaceae) was successively extracted with hexane, acetone, methanol and 70% methanol, and the extracts were further separated into a total of 21 fractions by silica gel or octadecylsilane (ODS) column chromatography. The biological activities of extracts and fractions were determined. These extracts showed relatively higher cytotoxic activity against two human oral tumor cell lines (HSC-2, HSG) than against normal human gingival fibroblasts (HGF), suggesting a tumor-specific cytotoxic activity. The cytotoxic activity of these extracts was enhanced by fractionation on silica gel [H2, A2, M1-M3] or ODS column chromatography [70M]. Several fractions [H2, H4, H5, A1, A2, A3, A5, A6, A7, M2] reversed the multidrug resistance (MDR) phenotype with L5178 mouse lymphoma T cells, more efficiently than (+/-)-verapamil. The extracts and fractions did not show any detectable anti-human immunodeficiency virus (HIV) or anti-Helicobacter pylori activity. Thus, this study suggests the effective and selective antitumor potential of 'Anastasia Red' of sweet pepper for further phytochemical and biological investigation. Copyright 2003 John Wiley & Sons, Ltd.

Laboratory evaluation of molluscicidal activity of extracts from Cotula cinerea (L) and Quercus lusitania var. infectoria galls (Oliv.).

PubMed

Redwane, A; Markouk, M; Lazrek, H B; Amarouch, H; Jana, M

1998-01-01

In this work, we have studied the molluscicidal activity of different extracts obtained from Cotula cinerea and Quercus lusitania var. infectoria galls. The hydroalcoholic extract of Cotula cinerea, acetonic extract and gallotanin of Quercus infectoria galls have presented high activity against Bulinus truncatus. The hydroalcoholic extract of Cotula cinerea was fractionated by chromatography on silica gel column. We have isolated two very active fractions at concentrations respectively of 52.5 and 27.5 ppm.

Sequential extraction procedure for determination of uranium, thorium, radium, lead and polonium radionuclides by alpha spectrometry in environmental samples

NASA Astrophysics Data System (ADS)

Oliveira, J. M.; Carvalho, F. P.

2006-01-01

A sequential extraction technique was developed and tested for common naturally-occurring radionuclides. This technique allows the extraction and purification of uranium, thorium, radium, lead, and polonium radionuclides from the same sample. Environmental materials such as water, soil, and biological samples can be analyzed for those radionuclides without matrix interferences in the quality of radioelement purification and in the radiochemical yield. The use of isotopic tracers (232U, 229Th, 224Ra, 209Po, and stable lead carrier) added to the sample in the beginning of the chemical procedure, enables an accurate control of the radiochemical yield for each radioelement. The ion extraction procedure, applied after either complete dissolution of the solid sample with mineral acids or co-precipitation of dissolved radionuclide with MnO2 for aqueous samples, includes the use of commercially available pre-packed columns from Eichrom® and ion exchange columns packed with Bio-Rad resins, in altogether three chromatography columns. All radioactive elements but one are purified and electroplated on stainless steel discs. Polonium is spontaneously plated on a silver disc. The discs are measured using high resolution silicon surface barrier detectors. 210Pb, a beta emitter, can be measured either through the beta emission of 210Bi, or stored for a few months and determined by alpha spectrometry through the in-growth of 210Po. This sequential extraction chromatography technique was tested and validated with the analysis of certified reference materials from the IAEA. Reproducibility was tested through repeated analysis of the same homogeneous material (water sample).

Intense laser pulse propagation in capillary discharge plasma channels

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

Hubbard, R. F.; Moore, C. I.; Sprangle, P.

Optical guiding of intense laser pulses is required for plasma-based accelerator concepts such as the laser wakefield accelerator. Reported experiments have successfully transported intense laser pulses in the hollow plasma column produced by a capillary discharge. The hollow plasma has an index of refraction which peaks on-axis, thus providing optical guiding which overcomes beam expansion due to diffraction. In more recent experiments at Hebrew University, 800 nm wavelength, 0.1 mJ, 100 fs pulses have been guided in {approx}300 micron radius capillaries over distances as long as 6.6 cm. Simulations of these experiments using a 2-D nonlinear laser propagation model producemore » the expected optical guiding, with the laser pulse radius r{sub L} exhibiting oscillations about the equilibrium value predicted by an analytical envelope equation model. The oscillations are damped at the front of the pulse and grow in amplitude in the back of the pulse. This growth and damping is attributed to finite pulse length effects. Simulations also show that further ionization of the discharge plasma by the laser pulse may hollow the laser pulse and introduce modulations in the spot size. This ionization-defocusing effect is expected to be significant at the high intensities required for accelerator application. Capillary discharge experiments at much higher intensities are in progress on the Naval Research Laboratory T{sup 3} laser, and preliminary results are reported.« less

Homogenization-assisted cavitation hybrid rotation extraction and macroporous resin enrichment of dihydroquercetin from Larix gmelinii.

PubMed

Xia, Yu; Wang, Yinhang; Li, Wei; Ma, Chunhui; Liu, Shouxin

2017-12-01

Cavitation hybrid rotation, which was and is still looked upon as an unavoidable nuisance in the flow systems, for extraction processing intensification of active chemical compounds from natural products. In this study, a homogenization-assisted cavitation hybrid rotation extraction method was applied to extract dihydroquercetin (DHQ) from larch (Larix gmelinii) wood root. The extraction parameters were optimized in single factor experiments with the DHQ extraction yields as the response values. The optimum conditions were as follows: number of extractions, three; ethanol volume fraction for the extraction, 60%; liquid-solid ratio for homogenization, 10mL/g; homogenization time, 8min; liquid-solid ratio for cavitation extraction, 9mL/g, and cavitation extraction time, 35min. Under these conditions, the DHQ content in extract was 4.50±0.02mg/g, and the extraction efficiency was higher than those of traditional techniques. Cavitation can be effectively used to improve the extraction rate by increasing the mass transfer rates and possible rupture of cell wall due to formation of microcavities leading to higher product yields with reduced processing time and solvent consumption. After the extraction process, macroporous resin column chromatography was used to concentrate and purify the DHQ. Three resins were selected from fifteen macroporous resins for further investigation of their performance. Among these resins, AB-8 resin exhibited relatively better adsorption capacities and desorption ratios for DHQ. The ethanol volume fraction of the solutions for sample loading and desorption, and flow rates for loading and desorption were optimized for the macroporous resin column chromatography. Copyright © 2017 Elsevier B.V. All rights reserved.

Sequential injection system with in-line solid phase extraction and soil mini-column for determination of zinc and copper in soil leachates.

PubMed

Paluch, Justyna; Mesquita, Raquel B R; Cerdà, Víctor; Kozak, Joanna; Wieczorek, Marcin; Rangel, António O S S

2018-08-01

A sequential injection (SI) system equipped with in-line solid phase extraction column and in-line soil mini-column is proposed for determination of zinc and copper in soil leachates. The spectrophotometric determination (560 nm) is based on the reaction of both analytes with 1-(2-Pyridylazo)-2-naphthol (PAN). Zinc is determined after retaining copper on a cationic resin (Chelex100) whereas copper is determined from the difference of the absorbance measured for both analytes, introduced into the system with the use of a different channel, and zinc absorbance. The influence of several potential interferences was studied. Using the developed method, zinc and copper were determined within the concentration ranges of 0.005-0.300 and 0.011-0.200 mg L -1 , and with a relative standard deviation lower than 6.0% and 5.1%, respectively. The detection limits are 1.4 and 3.0 µg/L for determination of zinc and copper, respectively. The developed SI method was verified by the determination of both analytes in synthetic and certified reference materials of water samples, and applied to the determination of the analytes in rain water and soil leachates from laboratory scale soil core column and in-line soil mini-column. Copyright © 2018 Elsevier B.V. All rights reserved.

From air to rubber: New techniques for measuring and replicating mouthpieces, bocals, and bores

NASA Astrophysics Data System (ADS)

Fuks, Leonardo

2002-11-01

The history of musical instruments comprises a long genealogy of models and prototypes that results from a combination of copying existing specimens with the change in constructive parameters, and the addition of new devices. In making wind instruments, several techniques have been traditionally employed for extracting the external and internal dimensions of toneholes, air columns, bells, and mouthpieces. In the twentieth century, methods such as pulse reflectometry, x-ray, magnetic resonance, and ultrasound imaging have been made available for bore measurement. Advantages and drawbacks of the existing methods are discussed and a new method is presented that makes use of the injection and coating of silicon rubber, for accurate molding of the instrument. This technique is harmless to all traditional materials, being indicated also for measurements of historical instruments. The paper presents dimensional data obtained from clarinet and saxophone mouthpieces. A set of replicas of top quality clarinet and saxophone mouthpieces, trombone bocals, and flute headjoints is shown, with comparative acoustical and performance analyses. The application of such techniques for historical and modern instrument analysis, restoration, and manufacturing is proposed.

Chromatographic column evaluation for the untargeted profiling of glucosinolates in cauliflower by means of ultra-high performance liquid chromatography coupled to high resolution mass spectrometry.

PubMed

Capriotti, Anna Laura; Cavaliere, Chiara; La Barbera, Giorgia; Montone, Carmela Maria; Piovesana, Susy; Zenezini Chiozzi, Riccardo; Laganà, Aldo

2018-03-01

The untargeted profiling is a promising approach for the characterization of secondary metabolites in biological matrices. Thanks to the recent rapid development of high-resolution mass spectrometry (HRMS) instrumentations, the number of applications by untargeted approaches for biological samples profiling has widely increased in the recent years. Despite the high potentialities of HRMS, however, a major issue in natural products analysis often arises in the upstream process of compounds separation. A separation technique is necessary to avoid phenomena such as signal suppression, and it is especially needed in the presence of isomeric metabolites, which are otherwise indistinguishable. Glucosinolates (GLSs), a group of secondary metabolites widely distributed among plants, resulted to be associated to the prevention of some serious diseases, such as cancer. This led to the development of several methods for the analysis of GLSs in vegetables tissues. The issue of GLSs chromatographic separation has been widely studied in the past because of the difficulty in the analysis of this highly polar and variable class of compounds. Several alternatives to reversed phase (RP) chromatography, sometimes not compatible with the coupling of liquid chromatography with mass spectrometry, have been tested for the analysis of intact GLSs. However, the availability of new stationary phases, in the last years, could allow the re-evaluation of RP chromatography for the analysis of intact GLSs. In this work, a thorough evaluation of four RP chromatographic columns for the analysis of GLSs in cauliflower (Brassica oleracea L. var. botrytis) extracts by an ultra-high performance liquid chromatographic system coupled via electrospray source to a hybrid quadrupole-Orbitrap mass spectrometer is presented. The columns tested were the following: one column Luna Omega polar C 18 , one column Kinetex Biphenyl, one column Kinetex core-shell XB-C 18 , two columns Kinetex core-shell XB-C 18 . After a previous optimization of the extraction method, cauliflower extracts were analyzed testing four different mobile phases onto the four columns for a total of sixteen different chromatographic conditions. The chromatographic systems were evaluated based on the number of detected and tentatively identified GLSs. Luna Polar stationary phase resulted to be the most suitable for the analysis of GLSs compared to Kinetex XB and Kinetex Biphenyl columns stationary phase. However, two in series Kinetex XB columns increased the number of tentatively identified GLSs compared to one Kinetex XB, showing the importance of column length in the analysis of complex mixtures. The data obtained with the best chromatographic system were deeply analyzed by MS/MS investigation for the final identification. Fiflty-one GLSs were tentatively identified, 24 of which have never been identified in cauliflower. Finally the linearity of the analytes response over the analyzed range of concentration was checked, suggesting that the developed method is suitable for both qualitative and quantitative analysis of GLSs in phytochemical mixtures. Copyright © 2017 Elsevier B.V. All rights reserved.

Formation of a spark discharge in an inhomogeneous electric field with current limitation by a large ballast Resistance

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

Baldanov, B. B., E-mail: baibat@mail.ru

2016-01-15

Results of studies of a spark discharge initiated in argon in a point–plane electrode gap with limitation of the discharge current by a large ballast resistance are presented. It is shown that the current flowing through the plasma channel of such a low-current spark has the form of periodic pulses. It is experimentally demonstrated that, when a low-current spark transforms into a constricted glow discharge, current pulses disappear, the spatial structure of the cathode glow changes abruptly, and a brightly glowing positive plasma column forms in the gap.

Running wavelet archetype aids the determination of heart rate from the video photoplethysmogram during motion.

PubMed

Addison, Paul S; Foo, David M H; Jacquel, Dominique

2017-07-01

The extraction of heart rate from a video-based biosignal during motion using a novel wavelet-based ensemble averaging method is described. Running Wavelet Archetyping (RWA) allows for the enhanced extraction of pulse information from the time-frequency representation, from which a video-based heart rate (HRvid) can be derived. This compares favorably to a reference heart rate derived from a pulse oximeter.

Super-pixel extraction based on multi-channel pulse coupled neural network

NASA Astrophysics Data System (ADS)

Xu, GuangZhu; Hu, Song; Zhang, Liu; Zhao, JingJing; Fu, YunXia; Lei, BangJun

2018-04-01

Super-pixel extraction techniques group pixels to form over-segmented image blocks according to the similarity among pixels. Compared with the traditional pixel-based methods, the image descripting method based on super-pixel has advantages of less calculation, being easy to perceive, and has been widely used in image processing and computer vision applications. Pulse coupled neural network (PCNN) is a biologically inspired model, which stems from the phenomenon of synchronous pulse release in the visual cortex of cats. Each PCNN neuron can correspond to a pixel of an input image, and the dynamic firing pattern of each neuron contains both the pixel feature information and its context spatial structural information. In this paper, a new color super-pixel extraction algorithm based on multi-channel pulse coupled neural network (MPCNN) was proposed. The algorithm adopted the block dividing idea of SLIC algorithm, and the image was divided into blocks with same size first. Then, for each image block, the adjacent pixels of each seed with similar color were classified as a group, named a super-pixel. At last, post-processing was adopted for those pixels or pixel blocks which had not been grouped. Experiments show that the proposed method can adjust the number of superpixel and segmentation precision by setting parameters, and has good potential for super-pixel extraction.

Extraction and analysis methods for the determination of pyrethroid insecticides in surface water, sediments and biological tissues at environmentally relevant concentrations.

PubMed

Mekebri, A; Crane, D B; Blondina, G J; Oros, D R; Rocca, J L

2008-05-01

The aim of this study was to develop and validate chemical methods for measuring pyrethroid insecticides at environmentally relevant concentrations in different matrices. The analytes included six synthetic pyrethroids with the highest agricultural and commercial structural uses in California: bifenthrin, cyfluthrin, cypermethrin, esfenvalerate/fenvalerate, lambda-cyhalothrin, permethrin, and their corresponding stereoisomers, which includes enantiomers, diastereomers and racemic mixtures. Fortified water samples were extracted for analysis of synthetic pyrethroids using liquid-liquid extraction, while fortified sediment and fish tissue samples were extracted using pressurized fluid extraction followed by gel permeation chromatography (GPC) to remove matrix interferences. A florisil column was used for additional cleanup and fractionation of sediment and tissue extracts. Extracts were analyzed using dual column high resolution gas chromatography with electron capture detection (GC/ECD) and confirmation was obtained with gas chromatography mass spectrometry using a quadrupole ion trap detector in MS-MS mode. Method detection limits (MDLs) have been established for water (1-3 ng/L), sediment (0.5-4 ng/g dry weight) and tissue (1-3 ng/g fresh weight). Mean percent recoveries of fortified blanks and samples ranged from 75 to 115% with relative standard deviation (RSD) values less than 20% for all target compounds.

Antioxidant Activity of a Red Lentil Extract and Its Fractions

PubMed Central

Amarowicz, Ryszard; Estrella, Isabell; Hernández, Teresa; Dueñas, Montserrat; Troszyńska, Agnieszka; Agnieszka, Kosińska; Pegg, Ronald B.

2009-01-01

Phenolic compounds were extracted from red lentil seeds using 80% (v/v) aqueous acetone. The crude extract was applied to a Sephadex LH-20 column. Fraction 1, consisting of sugars and low-molecular-weight phenolics, was eluted from the column by ethanol. Fraction 2, consisting of tannins, was obtained using acetone-water (1:1; v/v) as the mobile phase. Phenolic compounds present in the crude extract and its fractions demonstrated antioxidant and antiradical activities as revealed from studies using a β-carotene-linoleate model system, the total antioxidant activity (TAA) method, the DPPH radical-scavenging activity assay, and a reducing power evaluation. Results of these assays showed the highest values when tannins (fraction 2) were tested. For instance, the TAA of the tannin fraction was 5.85 μmol Trolox® eq./mg, whereas the crude extract and fraction 1 showed 0.68 and 0.33 μmol Trolox® eq./mg, respectively. The content of total phenolics in fraction 2 was the highest (290 mg/g); the tannin content, determined using the vanillin method and expressed as absorbance units at 500 nm per 1 g, was 129. There were 24 compounds identified in the crude extract using an HPLC-ESI-MS method: quercetin diglycoside, catechin, digallate procyanidin, and p-hydroxybenzoic were the dominant phenolics in the extract. PMID:20054484

High-throughput and selective solid-phase extraction of urinary catecholamines by crown ether-modified resin composite fiber.

PubMed

Chen, LiQin; Wang, Hui; Xu, Zhen; Zhang, QiuYue; Liu, Jia; Shen, Jun; Zhang, WanQi

2018-08-03

In the present study, we developed a simple and high-throughput solid phase extraction (SPE) procedure for selective extraction of catecholamines (CAs) in urine samples. The SPE adsorbents were electrospun composite fibers functionalized with 4-carboxybenzo-18-crown-6 ether modified XAD resin and polystyrene, which were packed into 96-well columns and used for high-throughput selective extraction of CAs in healthy human urine samples. Moreover, the extraction efficiency of packed-fiber SPE (PFSPE) was examined by high performance liquid chromatography coupled with fluorescence detector. The parameters affecting the extraction efficiency and impurity removal efficiency were optimized, and good linearity ranging from 0.5 to 400 ng/mL was obtained with a low limit of detection (LOD, 0.2-0.5 ng/mL) and a good repeatability (2.7%-3.7%, n = 6). The extraction recoveries of three CAs ranged from 70.5% to 119.5%. Furthermore, stable and reliable results obtained by the fluorescence detector were superior to those obtained by the electrochemical detector. Collectively, PFSPE coupled with 96-well columns was a simple, rapid, selective, high-throughput and cost-efficient method, and the proposed method could be applied in clinical chemistry. Copyright © 2018 Elsevier B.V. All rights reserved.

Lidar investigations of M-zone

NASA Technical Reports Server (NTRS)

Ovezgeldiyev, O. G.; Kurbanmuradov, K.; Lagutin, M. F.; Zarudny, A. A.; Meghel, Yu. E.; Torba, A. A.; Melnikov, V. E.

1987-01-01

The creation of pulse dye lasers tuned to resonant line of meteor produced admixtures of atmospheric constituents has made it possible to begin lidar investigations of the vertical distribution of mesospheric sodium concentration and its dynamics in the upper atmosphere. The observed morning increase of sodium concentration in the vertical column is probably caused by diurnal variations of sporadic meteors. The study of the dynamics of the sodium column concentration in the period of meteor streams activity confirms the suggestion of cosmic origin of these atoms. The short lived increase of sodium concentration brought about by a meteor stream, however, exceeds by one order the level of the sporadic background.

Changes to the Spectral Extraction Algorithm at the Third COS FUV Lifetime Position

NASA Astrophysics Data System (ADS)

Taylor, Joanna M.; Azalee Bostroem, K.; Debes, John H.; Ely, Justin; Hernandez, Svea; Hodge, Philip E.; Jedrzejewski, Robert I.; Lindsay, Kevin; Lockwood, Sean A.; Massa, Derck; Oliveira, Cristina M.; Penton, Steven V.; Proffitt, Charles R.; Roman-Duval, Julia; Sahnow, David J.; Sana, Hugues; Sonnentrucker, Paule

2015-01-01

Due to the effects of gain sag on flux on the COS FUV microchannel plate detector, the COS FUV spectra will be moved in February 2015 to a pristine location on the detector, from Lifetime Position 2 (LP2) to LP3. The spectra will be shifted in the cross-dispersion (XD) direction by -2.5", about -31 pixels, from the original LP1. In contrast, LP2 was shifted by +3.5", about 41 pixels, from LP1. By reducing the LP3-LP1 separation compared to the LP2-LP1 separation, we achieve maximal spectral resolution at LP3 while preserving more detector area for future lifetime positions. In the current version of the COS boxcar extraction algorithm, flux is summed within a box of fixed height that is larger than the PSF. Bad pixels located anywhere within the extraction box cause the entire column to be discarded. At the new LP3 position the current extraction box will overlap with LP1 regions of low gain (pixels which have lost >5% of their sensitivity). As a result, large portions of spectra will be discarded, even though these flagged pixels will be located in the wings of the profiles and contain a negligible fraction of the total source flux. To avoid unnecessarily discarding columns affected by such pixels, an algorithm is needed that can judge whether the effects of gain-sagged pixels on the extracted flux are significant. The "two-zone" solution adopted for pipeline use was tailored specifically for the COS FUV data characteristics: First, using a library of 1-D spectral centroid ("trace") locations, residual geometric distortions in the XD direction are removed. Next, 2-D template profiles are aligned with the observed spectral image. Encircled energy contours are calculated and an inner zone that contains 80% of the flux is defined, as well as an outer zone that contains 99% of the flux. With this approach, only pixels flagged as bad in the inner 80% zone will cause columns to be discarded while flagged pixels in the outer zones do not affect extraction. Finally, all good columns are summed in the XD direction to obtain a 1-D extracted spectrum. We present examples of the trace and profile libraries that are used in the two-zone extraction and compare the performance of the two-zone and boxcar algorithms.

Anti-diabetic property of Methanol extract of Musa sapientum leaves and its fractions in alloxan-induced diabetic rats.

PubMed

Adewoye, E O; Ige, A O

2013-06-30

Diabetes mellitus is a metabolic disorder resulting from necrosis of β-cell and insulin resistance at the cellular level. Musa sapientum has been shown to possess anti-diabetic properties, however, the mechanism of its action is unknown. The effect of Methanolic extract of Musa sapientum leaves (MEMSL) and its fractions were assessed for in vitro inhibitory activity of α-amylase enzyme, in vivo hypoglycemic properties and liver glycogen content in alloxan-induced diabetic rats. Dried plant powder of Musa sapientum was successively extracted using n-hexane, ethyl acetate, dichloromethane and methanol respectively. The filtrate obtained was evaporated using rotary evaporator and the extract was stored at 4°C until use. The methanolic extract obtained was further fractionated using column chromatography. In vitro alpha amylase inhibitory activity of the methanolic extract at different doses (2.5mg/ml, 5mg/ml, 10mg/ml, 25mg/ml and 50mg/ml) and column fractions (100ug/ml) were assessed and compared with that of acarbose (5mg/ml), a standard oral α-amylase inhibitor. Hypoglycemic activity and liver glycogen content was studied using alloxan -induced diabetic male rats treated with MEMSL (250mg/kg and 500mg/kg), column fractions F2 and F5 (100μg/kg) for 14 days respectively. Results obtained showed a dose -dependent increase in α-amylase inhibitory activity of the methanolic extract at 5, 10, 25 and 50mg/ml exhibiting 29%, 61%, and 72% and 80% inhibitory activities respectively. Column fractions 2 and 5 showed the highest α-amylase inhibitory activity of 79% and 74% respectively. The MEMSL at 250mg/kg and 500mg/kg exhibited 66% and 59% hypoglycemic activities respectively compared with diabetic controls. Fractions 2 and 5 showed 48% and 75% reduction in blood glucose level respectively. Liver glycogen in diabetic animals treated with MEMSL (250mg/kg and 500mg/kg), F2 and F5 were significantly increased (5.5±0.5, 5.9±0.7, 3.6±0.5, 8.0±0.4 mg/100gwt. liver) compared with Diabetic controls (1.2±0.3 mg/100gwt. liver) respectively suggesting an increase in glucose storage or reduction in glycogen breakdown. It seems possible that the anti-diabetic properties in the leaf extract of Musa sapientum and its fractions maybe due to the inhibition of α-amylase, increased storage of glucose as glycogen in the liver and/or reduced breakdown of liver glycogen stores.

SGR 1822-1606: Constant Spin Period

NASA Astrophysics Data System (ADS)

Serim, M.; Baykal, A.; Inam, S. C.

2011-08-01

We have analyzed light curve of the new source SGR 1822-1606 (Cummings et al. GCN 12159) using the real time data of RXTE observations. We have extracted light curve for 11 pointings with a time span of about 20 days and employed pulse timing analysis using the harmonic representation of pulses. Using the cross correlation of harmonic representation of pulses, we have obtained pulse arrival times.

Knee cartilage extraction and bone-cartilage interface analysis from 3D MRI data sets

NASA Astrophysics Data System (ADS)

Tamez-Pena, Jose G.; Barbu-McInnis, Monica; Totterman, Saara

2004-05-01

This works presents a robust methodology for the analysis of the knee joint cartilage and the knee bone-cartilage interface from fused MRI sets. The proposed approach starts by fusing a set of two 3D MR images the knee. Although the proposed method is not pulse sequence dependent, the first sequence should be programmed to achieve good contrast between bone and cartilage. The recommended second pulse sequence is one that maximizes the contrast between cartilage and surrounding soft tissues. Once both pulse sequences are fused, the proposed bone-cartilage analysis is done in four major steps. First, an unsupervised segmentation algorithm is used to extract the femur, the tibia, and the patella. Second, a knowledge based feature extraction algorithm is used to extract the femoral, tibia and patellar cartilages. Third, a trained user corrects cartilage miss-classifications done by the automated extracted cartilage. Finally, the final segmentation is the revisited using an unsupervised MAP voxel relaxation algorithm. This final segmentation has the property that includes the extracted bone tissue as well as all the cartilage tissue. This is an improvement over previous approaches where only the cartilage was segmented. Furthermore, this approach yields very reproducible segmentation results in a set of scan-rescan experiments. When these segmentations were coupled with a partial volume compensated surface extraction algorithm the volume, area, thickness measurements shows precisions around 2.6%

Determination of linuron and related compounds in soil by microwave-assisted solvent extraction and reversed-phase liquid chromatography with UV detection.

PubMed

Molins, C; Hogendoorn, E A; Dijkman, E; Heusinkveld, H A; Baumann, R A

2000-02-11

The combination of microwave-assisted solvent extraction (MASE) and reversed-phase liquid chromatography (RPLC) with UV detection has been investigated for the efficient determination of phenylurea herbicides in soils involving the single-residue method (SRM) approach (linuron) and the multi-residue method (MRM) approach (monuron, monolinuron, isoproturon, metobromuron, diuron and linuron). Critical parameters of MASE, viz, extraction temperature, water content and extraction solvent were varied in order to optimise recoveries of the analytes while simultaneously minimising co-extraction of soil interferences. The optimised extraction procedure was applied to different types of soil with an organic carbon content of 0.4-16.7%. Besides freshly spiked soil samples, method validation included the analysis of samples with aged residues. A comparative study between the applicability of RPLC-UV without and with the use of column switching for the processing of uncleaned extracts, was carried out. For some of the tested analyte/matrix combinations the one-column approach (LC mode) is feasible. In comparison to LC, coupled-column LC (LC-LC mode) provides high selectivity in single-residue analysis (linuron) and, although less pronounced in multi-residue analysis (all six phenylurea herbicides), the clean-up performance of LC-LC improves both time of analysis and sample throughput. In the MRM approach the developed procedure involving MASE and LC-LC-UV provided acceptable recoveries (range, 80-120%) and RSDs (<12%) at levels of 10 microg/kg (n=9) and 50 microg/kg (n=7), respectively, for most analyte/matrix combinations. Recoveries from aged residue samples spiked at a level of 100 microg/kg (n=7) ranged, depending of the analyte/soil type combination, from 41-113% with RSDs ranging from 1-35%. In the SRM approach the developed LC-LC procedure was applied for the determination of linuron in 28 sandy soil samples collected in a field study. Linuron could be determined in soil with a limit of quantitation of 10 microg/kg.

Pulsed ultraviolet light reduces immunoglobulin E binding to Atlantic white shrimp (Litopenaeus setiferus) extract.

PubMed

Shriver, Sandra; Yang, Wade; Chung, Si-Yin; Percival, Susan

2011-07-01

Pulsed ultraviolet light (PUV), a novel food processing and preservation technology, has been shown to reduce allergen levels in peanut and soybean samples. In this study, the efficacy of using PUV to reduce the reactivity of the major shrimp allergen, tropomyosin (36-kDa), and to attenuate immunoglobulin E (IgE) binding to shrimp extract was examined. Atlantic white shrimp (Litopenaeus setiferus) extract was treated with PUV (3 pulses/s, 10 cm from light source) for 4 min. Tropomyosin was compared in the untreated, boiled, PUV-treated and [boiled+PUV]-treated samples, and changes in the tropomyosin levels were determined by sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE). IgE binding of the treated extract was analyzed via immunoblot and enzyme-linked immunosorbent assay (ELISA) using pooled human plasma containing IgE antibodies against shrimp allergens. Results showed that levels of tropomyosin and IgE binding were reduced following PUV treatment. However, boiling increased IgE binding, while PUV treatment could offset the increased allergen reactivity caused by boiling. In conclusion, PUV treatment reduced the reactivity of the major shrimp allergen, tropomyosin, and decreased the IgE binding capacity of the shrimp extract.

Application of acoustic doppler current profilers for measuring three-dimensional flow fields and as a surrogate measurement of bedload transport

USGS Publications Warehouse

Conaway, Jeffrey S.

2005-01-01

Acoustic Doppler current profilers (ADCPs) have been in use in the riverine environment for nearly 20 years. Their application primarily has been focused on the measurement of streamflow discharge. ADCPs emit high-frequency sound pulses and receive reflected sound echoes from sediment particles in the water column. The Doppler shift between transmitted and return signals is resolved into a velocity component that is measured in three dimensions by simultaneously transmitting four independent acoustical pulses. To measure the absolute velocity magnitude and direction in the water column, the velocity magnitude and direction of the instrument must also be computed. Typically this is accomplished by ensonifying the streambed with an acoustical pulse that also provides a depth measurement for each of the four acoustic beams. Sediment transport on or near the streambed will bias these measurements and requires external positioning such as a differentially corrected Global Positioning Systems (GPS). Although the influence of hydraulic structures such as spur dikes and bridge piers is typically only measured and described in one or two dimensions, the use of differentially corrected GPS with ADCPs provides a fully three-dimensional measurement of the magnitude and direction of the water column at such structures. The measurement of these flow disturbances in a field setting also captures the natural pulsations of river flow that cannot be easily quantified or modeled by numerical simulations or flumes. Several examples of measured three-dimensional flow conditions at bridge sites throughout Alaska are presented. The bias introduced to the bottom-track measurement is being investigated as a surrogate measurement of bedload transport. By fixing the position of the ADCP for a known period of time the apparent velocity of the streambed at that position can be determined. Initial results and comparison to traditionally measured bedload values are presented. These initial results and those by other researchers are helping to determine a direction for further research of noncontact measurements of sediment transport. Copyright ASCE 2005.

Response of Soil Biogeochemistry to Freeze-thaw Cycles: Impacts on Greenhouse Gas Emission and Nutrient Fluxes

NASA Astrophysics Data System (ADS)

Rezanezhad, F.; Parsons, C. T.; Smeaton, C. M.; Van Cappellen, P.

2014-12-01

Freeze-thaw is an abiotic stress applied to soils and is a natural process at medium to high latitudes. Freezing and thawing processes influence not only the physical properties of soil, but also the metabolic activity of soil microorganisms. Fungi and bacteria play a crucial role in soil organic matter degradation and the production of greenhouse gases (GHG) such as CO2, CH4 and N2O. Production and consumption of these atmospheric trace gases are the result of biological processes such as photosynthesis, aerobic respiration (CO2), methanogenesis, methanotrophy (CH4), nitrification and denitrification (N2O). To enhance our understanding of the effects of freeze-thaw cycles on soil biogeochemical transformations and fluxes, a highly instrumented soil column experiment was designed to realistically simulate freeze-thaw dynamics under controlled conditions. Pore waters collected periodically from different depths of the column and solid-phase analyses on core material obtained at the initial and end of the experiment highlighted striking geochemical cycling. CO2, CH4 and N2O production at different depths within the column were quantified from dissolved gas concentrations in pore water. Subsequent emissions from the soil surface were determined by direct measurement in the head space. Pulsed CO2 emission to the headspace was observed at the onset of thawing, however, the magnitude of the pulse decreased with each subsequent freeze-thaw cycle indicating depletion of a "freeze-thaw accessible" carbon pool. Pulsed CO2 emission was due to a combination of physical release of gases dissolved in porewater and entrapped below the frozen zone and changing microbial respiration in response to electron acceptor variability (O2, NO3-, SO42-). In this presentation, we focus on soil-specific physical, chemical, microbial factors (e.g. redox conditions, respiration, fermentation) and the mechanisms that drive GHG emission and nutrient cycling in soils under freeze-thaw cycles.

Migration through soil of organic solutes in an oil-shale process water

USGS Publications Warehouse

Leenheer, J.A.; Stuber, H.A.

1981-01-01

The migration through soil of organic solutes in an oil-shale process water (retort water) was studied by using soil columns and analyzing leachates for various organic constituents. Retort water extracted significant quantities of organic anions leached from ammonium-saturated-soil organic matter, and a distilled-water rinse, which followed retort-water leaching, released additional organic acids from the soil. After being corrected for organic constitutents extracted from soil by retort water, dissolved-organic-carbon fractionation analyses of effluent fractions showed that the order of increasing affinity of six organic compound classes for the soil was as follows: hydrophilic neutrals nearly equal to hydrophilic acids, followed by the sequence of hydrophobic acids, hydrophilic bases, hydrophobic bases, and hydrophobic neutrals. Liquid-chromatographic analysis of the aromatic amines in the hydrophobic- and hydrophilic-base fractions showed that the relative order of the rates of migration through the soil column was the same as the order of migration on a reversed-phase, octadecylsilica liquid-chromatographic column.

Bonded-phase extraction column isolation of organic compounds in groundwater at a hazardous waste site

USGS Publications Warehouse

Rostad, C.E.; Pereira, W.E.; Ratcliff, S.M.

1984-01-01

A procedure for isolation of hazardous organic compounds from water for gas chromatography/mass spectrometry analysis Is presented and applied to creosote- and pentachlorophenol-contaminated groundwater resulting from wood-treatment processes. This simple procedure involved passing a 50-100-mL sample through a bonded-phase extraction column, eluting the trapped organic compounds from the column with 2-4 mL of solvent, and evaporating the sample to 100 ??L with a stream of dry nitrogen, after which the sample was ready for gas chromatography/mass spectrometry analysis. Representative compounds indicative of creosote contamination were used for recovery and precision studies from the cyclohexyl-bonded phase. Recovery of these compounds from n-octyl-, n-octadecyl-, cyclohexyl-, and phenyl-bonded phases was compared. The bonded phase that exhibited the best recovery and least bias toward acidic or basic cmpounds was the n-octadecyl phase. Detailed compound Identification Is given for compounds Isolated from creosote- and pentachlorophenol-contaminated groundwater using the cyclohexyl-bonded phase.

Responses of microbial community to pH stress in bioleaching of low grade copper sulfide.

PubMed

Wang, Yuguang; Li, Kai; Chen, Xinhua; Zhou, Hongbo

2018-02-01

The microbial diversity and dynamics in the leachates and on the ore surfaces of different depth of the column were analyzed during bioleaching of low grade copper sulfide at different pH, after inoculation with the same inoculum containing mesophiles and moderate thermophiles. The results indicate that low pH was beneficial to enhance copper extraction. The highest copper extraction (86%) was obtained when pH was controlled at 1.0-1.5. The microbial structures on the ore surfaces were independent of community structures in the leachate, even at the top portion of column. Microbial richness and evenness increased with decreasing pH during bioleaching. pH had significant effects on microbial community structure in the leachate and on the mineral surface of different depth of the column. Leptospirillum ferriphilum accounted for the highest proportions of the community at most times when pH was operated during bioleaching, especially at the end of run. Copyright © 2017 Elsevier Ltd. All rights reserved.

Phytochemical investigation on leaf extract of Cordia salicifolia Cham.

PubMed

Menghini, Luigi; Epifano, Francesco; Leporini, Lidia; Pagiotti, Rita; Tirillini, Bruno

2008-03-01

The dichloromethane extract of leaves of Cordia salicifolia Cham. (Family Boraginaceae) was fractionated by SiO(2) column chromatography and analyzed by gas chromatography, gas chromatography-mass spectrometry, and nuclear magnetic resonance spectroscopy. The apolar extract is characterized by a very high content of (+)-spathulenol (0.53%). The major component of the extract exhibited a very weak activity as an inhibitor of growth of Helicobacter pylori in vitro (minimum inhibitory concentration = 200 microg/mL).

Effect of chemical and physical heterogeneities on colloid-facilitated cesium transport

DOE PAGES

Rod, Kenton; Um, Wooyong; Chun, Jaehun; ...

2018-03-31

A set of column experiments was conducted to investigate the chemical and physical heterogeneity effect on colloid facilitated transport under slow pore velocity conditions. Pore velocities were kept below 100 cm d -1 for all experiments. Glass beads were packed into columns establishing four different conditions: 1) homogeneous, 2) mixed physical heterogeneity, 3) sequentially layered physical heterogeneity, and 4) chemical heterogeneity. The homogeneous column was packed with glass beads (diameter 500–600 μm), and physical heterogeneities were created by sequential layering or mixing two sizes of glass bead (500–600 μm and 300–400 μm). A chemical heterogeneity was created using 25% ofmore » the glass beads coated with hydrophobic molecules (1H-1H-2H-2H-perfluorooctyltrichlorosilane) mixed with 75% pristine glass beads (all 500–600 μm). Input solution with 0.5 mM CsI and 50 mg L -1 colloids (1-μm diameter SiO 2) was pulsed into columns under saturated conditions. The physical heterogeneity in the packed glass beads retarded the transport of colloids compared to homogeneous (R = 25.0), but showed only slight differences between sequentially layered (R = 60.7) and mixed heterogeneity(R = 62.4). The column with the chemical, hydrophobic/hydrophilic, heterogeneity removed most of the colloids from the input solution. All column conditions stripped Cs from colloids onto the column matrix of packed glass beads.« less

Effect of chemical and physical heterogeneities on colloid-facilitated cesium transport

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

Rod, Kenton; Um, Wooyong; Chun, Jaehun

A set of column experiments was conducted to investigate the chemical and physical heterogeneity effect on colloid facilitated transport under slow pore velocity conditions. Pore velocities were kept below 100 cm d -1 for all experiments. Glass beads were packed into columns establishing four different conditions: 1) homogeneous, 2) mixed physical heterogeneity, 3) sequentially layered physical heterogeneity, and 4) chemical heterogeneity. The homogeneous column was packed with glass beads (diameter 500–600 μm), and physical heterogeneities were created by sequential layering or mixing two sizes of glass bead (500–600 μm and 300–400 μm). A chemical heterogeneity was created using 25% ofmore » the glass beads coated with hydrophobic molecules (1H-1H-2H-2H-perfluorooctyltrichlorosilane) mixed with 75% pristine glass beads (all 500–600 μm). Input solution with 0.5 mM CsI and 50 mg L -1 colloids (1-μm diameter SiO 2) was pulsed into columns under saturated conditions. The physical heterogeneity in the packed glass beads retarded the transport of colloids compared to homogeneous (R = 25.0), but showed only slight differences between sequentially layered (R = 60.7) and mixed heterogeneity(R = 62.4). The column with the chemical, hydrophobic/hydrophilic, heterogeneity removed most of the colloids from the input solution. All column conditions stripped Cs from colloids onto the column matrix of packed glass beads.« less

Modular continuous wavelet processing of biosignals: extracting heart rate and oxygen saturation from a video signal

PubMed Central

2016-01-01

A novel method of extracting heart rate and oxygen saturation from a video-based biosignal is described. The method comprises a novel modular continuous wavelet transform approach which includes: performing the transform, undertaking running wavelet archetyping to enhance the pulse information, extraction of the pulse ridge time–frequency information [and thus a heart rate (HRvid) signal], creation of a wavelet ratio surface, projection of the pulse ridge onto the ratio surface to determine the ratio of ratios from which a saturation trending signal is derived, and calibrating this signal to provide an absolute saturation signal (SvidO2). The method is illustrated through its application to a video photoplethysmogram acquired during a porcine model of acute desaturation. The modular continuous wavelet transform-based approach is advocated by the author as a powerful methodology to deal with noisy, non-stationary biosignals in general. PMID:27382479

Electrically Variable Resistive Memory Devices

NASA Technical Reports Server (NTRS)

Liu, Shangqing; Wu, Nai-Juan; Ignatiev, Alex; Charlson, E. J.

2010-01-01

Nonvolatile electronic memory devices that store data in the form of electrical- resistance values, and memory circuits based on such devices, have been invented. These devices and circuits exploit an electrically-variable-resistance phenomenon that occurs in thin films of certain oxides that exhibit the colossal magnetoresistive (CMR) effect. It is worth emphasizing that, as stated in the immediately preceding article, these devices function at room temperature and do not depend on externally applied magnetic fields. A device of this type is basically a thin film resistor: it consists of a thin film of a CMR material located between, and in contact with, two electrical conductors. The application of a short-duration, low-voltage current pulse via the terminals changes the electrical resistance of the film. The amount of the change in resistance depends on the size of the pulse. The direction of change (increase or decrease of resistance) depends on the polarity of the pulse. Hence, a datum can be written (or a prior datum overwritten) in the memory device by applying a pulse of size and polarity tailored to set the resistance at a value that represents a specific numerical value. To read the datum, one applies a smaller pulse - one that is large enough to enable accurate measurement of resistance, but small enough so as not to change the resistance. In writing, the resistance can be set to any value within the dynamic range of the CMR film. Typically, the value would be one of several discrete resistance values that represent logic levels or digits. Because the number of levels can exceed 2, a memory device of this type is not limited to binary data. Like other memory devices, devices of this type can be incorporated into a memory integrated circuit by laying them out on a substrate in rows and columns, along with row and column conductors for electrically addressing them individually or collectively.

Continuous and pulsed ultrasound-assisted extractions of antioxidants from pomegranate peel

USDA-ARS?s Scientific Manuscript database

There is a great demand for developing efficient extraction methods in order to reduce extraction time and increase the yield and activity of functional antioxidants. The yields, activities, and extraction kinetics of antioxidants from dry peel of pomegranate marc were studied using ultrasound assis...

Continuous and pulsed ultrasound-assisted extractions of antioxidants from pomegranate peel

USDA-ARS?s Scientific Manuscript database

There is a great demand for developing efficient extraction methods in order to reduce extraction time and increase the yield and activity of functional antioxidants. The yields, activities, and extraction kinetics of antioxidants from dry peel of pomegranate marc were studied using ultrasound-assis...

HOMFLY for twist knots and exclusive Racah matrices in representation [333

NASA Astrophysics Data System (ADS)

Morozov, A.

2018-03-01

Next step is reported in the program of Racah matrices extraction from the differential expansion of HOMFLY polynomials for twist knots: from the double-column rectangular representations R = [ rr ] to a triple-column and triple-hook R = [ 333 ]. The main new phenomenon is the deviation of the particular coefficient f[ 332 ][ 21 ] from the corresponding skew dimension, what opens a way to further generalizations.

Analysis and Recognition of Traditional Chinese Medicine Pulse Based on the Hilbert-Huang Transform and Random Forest in Patients with Coronary Heart Disease

PubMed Central

Wang, Yiqin; Yan, Hanxia; Yan, Jianjun; Yuan, Fengyin; Xu, Zhaoxia; Liu, Guoping; Xu, Wenjie

2015-01-01

Objective. This research provides objective and quantitative parameters of the traditional Chinese medicine (TCM) pulse conditions for distinguishing between patients with the coronary heart disease (CHD) and normal people by using the proposed classification approach based on Hilbert-Huang transform (HHT) and random forest. Methods. The energy and the sample entropy features were extracted by applying the HHT to TCM pulse by treating these pulse signals as time series. By using the random forest classifier, the extracted two types of features and their combination were, respectively, used as input data to establish classification model. Results. Statistical results showed that there were significant differences in the pulse energy and sample entropy between the CHD group and the normal group. Moreover, the energy features, sample entropy features, and their combination were inputted as pulse feature vectors; the corresponding average recognition rates were 84%, 76.35%, and 90.21%, respectively. Conclusion. The proposed approach could be appropriately used to analyze pulses of patients with CHD, which can lay a foundation for research on objective and quantitative criteria on disease diagnosis or Zheng differentiation. PMID:26180536

Analysis and Recognition of Traditional Chinese Medicine Pulse Based on the Hilbert-Huang Transform and Random Forest in Patients with Coronary Heart Disease.

PubMed

Guo, Rui; Wang, Yiqin; Yan, Hanxia; Yan, Jianjun; Yuan, Fengyin; Xu, Zhaoxia; Liu, Guoping; Xu, Wenjie

2015-01-01

Objective. This research provides objective and quantitative parameters of the traditional Chinese medicine (TCM) pulse conditions for distinguishing between patients with the coronary heart disease (CHD) and normal people by using the proposed classification approach based on Hilbert-Huang transform (HHT) and random forest. Methods. The energy and the sample entropy features were extracted by applying the HHT to TCM pulse by treating these pulse signals as time series. By using the random forest classifier, the extracted two types of features and their combination were, respectively, used as input data to establish classification model. Results. Statistical results showed that there were significant differences in the pulse energy and sample entropy between the CHD group and the normal group. Moreover, the energy features, sample entropy features, and their combination were inputted as pulse feature vectors; the corresponding average recognition rates were 84%, 76.35%, and 90.21%, respectively. Conclusion. The proposed approach could be appropriately used to analyze pulses of patients with CHD, which can lay a foundation for research on objective and quantitative criteria on disease diagnosis or Zheng differentiation.

Regulated bioanalysis of conformers - A case study with ASP2151 in dog plasma and urine.

PubMed

Ohtsu, Yoshiaki; Otsuka, Shohei; Nakamura, Takeshi; Noguchi, Kiyoshi

2015-08-01

We developed and validated bioanalytical methods for a potent helicase-primase inhibitor ASP2151 that has two conformers. These conformers elute as unseparated broad peaks under ordinary high-performance liquid chromatographic conditions, indicating discernable differences in hydrophobicity. We observed that column temperature and mobile phase pH have no effect on these peaks and that conformers form a single symmetrical peak when tetrahydrofuran is added to the mobile phase. In addition, we needed to develop semi-automated methods where inter-conversion of the conformers is unlikely to cause sample-to-sample extraction variability. Briefly, following the addition of deuterium-labeled ASP2151 as an internal standard (IS), dog plasma samples or acetonitrile-added urine samples were filtrated. The filtrates were then injected into a column-switching liquid chromatography-tandem mass spectrometry (LC-MS/MS) system and trapped onto an extraction column. Extracts were back-flushed onto an analytical C18 column (4.6×50mm, 3μm) with a mobile phase consisting of methanol, tetrahydrofuran, and 20mmol/L ammonium acetate (45:5:50, v/v/v). The eluent was monitored in the negative atmospheric pressure chemical ionization mode. The calibration curve was linear over a range of 5-1000ng/mL for plasma and 0.5-100μg/mL for urine. Validation data met the acceptance criteria in accordance with regulatory guidance and demonstrated that these methods were selective, accurate, and reproducible. In addition, the present methods were successfully applied to a pharmacokinetic study in dogs. Copyright © 2015 Elsevier B.V. All rights reserved.

Transport of U(VI) through sediments amended with phosphate to induce in situ uranium immobilization.

PubMed

Mehta, Vrajesh S; Maillot, Fabien; Wang, Zheming; Catalano, Jeffrey G; Giammar, Daniel E

2015-02-01

Phosphate amendments can be added to U(VI)-contaminated subsurface environments to promote in situ remediation. The primary objective of this study was to evaluate the impacts of phosphate addition on the transport of U(VI) through contaminated sediments. In batch experiments using sediments (<2 mm size fraction) from a site in Rifle, Colorado, U(VI) only weakly adsorbed due to the dominance of the aqueous speciation by Ca-U(VI)-carbonate complexes. Column experiments with these sediments were performed with flow rates that correspond to a groundwater velocity of 1.1 m/day. In the absence of phosphate, the sediments took up 1.68-1.98 μg U/g of sediments when the synthetic groundwater influent contained 4 μM U(VI). When U(VI)-free influents were then introduced with and without phosphate, substantially more uranium was retained within the column when phosphate was present in the influent. Sequential extractions of sediments from the columns revealed that uranium was uniformly distributed along the length of the columns and was primarily in forms that could be extracted by ion exchange and contact with a weak acid. Laser induced fluorescence spectroscopy (LIFS) analysis along with sequential extraction results suggest adsorption as the dominant uranium uptake mechanism. The response of dissolved uranium concentrations to stopped-flow events and the comparison of experimental data with simulations from a simple reactive transport model indicated that uranium adsorption to and desorption from the sediments was not always at local equilibrium. Copyright © 2014 Elsevier Ltd. All rights reserved.

Fast analysis of curcuminoids from turmeric (Curcuma longa L.) by high-performance liquid chromatography using a fused-core column.

PubMed

Osorio-Tobón, J Felipe; Carvalho, Pedro I N; Barbero, Gerardo Fernández; Nogueira, Gislaine Chrystina; Rostagno, Mauricio Ariel; Meireles, Maria Angela de Almeida

2016-06-01

The recent development of fused-core technology in HPLC columns is enabling faster and highly efficient separations. This technology was evaluated for the development of a fast method for the analysis of main curcuminoids (curcumin, demethoxycurcumin and bisdemethoxycurcumin) present in extracts of turmeric (Curcuma longa L.). A step-by-step strategy was used to optimize temperature (40-55 °C), flow rate (1.0-2.5 mL min(-1)), mobile phase composition and equilibration time (1-5 min). A gradient method was developed using acidified water and acetonitrile combined with high column temperature (55 °C) and flow rate (2.5 mL min(-1)). Optimized conditions provided a method for the separation of these three curcuminoids in approximately 1.3 min with a total analysis time (sample-to-sample) of 7 min, including the clean-up and the re-equilibration of the column. Evaluation of chromatographic performance revealed excellent intraday and interday reproducibility (>99%), resolution (>2.23), selectivity (>1.12), peak symmetry (1.24-1.42) while presenting low limits of detection (<0.40 mg L(-1)) and quantification (<1.34 mg L(-1)). The robustness of the method was calculated according to the concentration/dilution of the sample and the injection volume. Several combinations of methanol and ethanol with water as sample solvents were evaluated and the best chromatographic results and extraction rate were obtained using 100% methanol. Finally, the developed method was validated with different extracts of turmeric rhizome and products that use turmeric in their formulation. Copyright © 2016 Elsevier Ltd. All rights reserved.

Comparison of salivary collection and processing methods for quantitative HHV-8 detection.

PubMed

Speicher, D J; Johnson, N W

2014-10-01

Saliva is a proved diagnostic fluid for the qualitative detection of infectious agents, but the accuracy of viral load determinations is unknown. Stabilising fluids impede nucleic acid degradation, compared with collection onto ice and then freezing, and we have shown that the DNA Genotek P-021 prototype kit (P-021) can produce high-quality DNA after 14 months of storage at room temperature. Here we evaluate the quantitative capability of 10 collection/processing methods. Unstimulated whole mouth fluid was spiked with a mixture of HHV-8 cloned constructs, 10-fold serial dilutions were produced, and samples were extracted and then examined with quantitative PCR (qPCR). Calibration curves were compared by linear regression and qPCR dynamics. All methods extracted with commercial spin columns produced linear calibration curves with large dynamic range and gave accurate viral loads. Ethanol precipitation of the P-021 does not produce a linear standard curve, and virus is lost in the cell pellet. DNA extractions from the P-021 using commercial spin columns produced linear standard curves with wide dynamic range and excellent limit of detection. When extracted with spin columns, the P-021 enables accurate viral loads down to 23 copies μl(-1) DNA. The quantitative and long-term storage capability of this system makes it ideal for study of salivary DNA viruses in resource-poor settings. © 2013 John Wiley & Sons A/S. Published by John Wiley & Sons Ltd.

A Non-thermal Pulsed X-Ray Emission of AR Scorpii

NASA Astrophysics Data System (ADS)

Takata, J.; Hu, C.-P.; Lin, L. C. C.; Tam, P. H. T.; Pal, P. S.; Hui, C. Y.; Kong, A. K. H.; Cheng, K. S.

2018-02-01

We report the analysis result of UV/X-ray emission from AR Scorpii, which is an intermediate polar (IP) composed of a magnetic white dwarf and an M-type star, with the XMM-Newton data. The X-ray/UV emission clearly shows a large variation over the orbit, and their intensity maximum (or minimum) is located at the superior conjunction (or inferior conjunction) of the M star orbit. The hardness ratio of the X-ray emission shows a small variation over the orbital phase and shows no indication of the absorption by an accretion column. These properties are naturally explained by the emission from the M star surface rather than that from the accretion column on the white dwarf’s (WD) star, which is similar to usual IPs. Additionally, the observed X-ray emission also modulates with the WD’s spin with a pulse fraction of ∼14%. The peak position is aligned in the optical/UV/X-ray band. This supports the hypothesis that the electrons in AR Scorpii are accelerated to a relativistic speed and emit non-thermal photons via the synchrotron radiation. In the X-ray bands, evidence of the power-law spectrum is found in the pulsed component, although the observed emission is dominated by the optically thin thermal plasma emissions with several different temperatures. It is considered that the magnetic dissipation/reconnection process on the M star surface heats up the plasma to a temperature of several keV and also accelerates the electrons to the relativistic speed. The relativistic electrons are trapped in the WD’s closed magnetic field lines by the magnetic mirror effect. In this model, the observed pulsed component is explained by the emissions from the first magnetic mirror point.

Radio Frequency Radiation Dosimetry Handbook (Fifth Edition)

DTIC Science & Technology

2009-07-01

the capacitance of the load . Assuming that the pulse shape is perfectly rectangular, the power dissipation in the sample during the pulse can be...microwave pulses at 2.37 GHz: No effect on vigilance performance in monkeys. Joint Naval Aerospace Medical Research Laboratory Research Report, NAMRL...Klauenberg, B. J., & Erwin, D. N. (1989). Lack of behavioral effects of high-peak-power microwave pulses from an axially extracted virtual cathode

Columnar Transitions in Microscale Evaporating Liquid Jets

NASA Astrophysics Data System (ADS)

Hunter, Hanif; Glezer, Ari

2007-11-01

Microscale evaporating liquid jets that are injected into a quiescent gaseous medium having adjustable ambient pressure are investigated over a range of jet speeds using a shadowgraph technique. The jets are formed by a laser-drilled 10 μm nozzle from a small-scale pressurized reservoir, and sub-atmospheric ambient pressure is maintained using a controllable, metered Venturi pump. The near-field jet features are captured by shadowgraph imaging using a pulsed ND-Yag laser and a 12 bit CCD camera where the field of view measured 200 μm on the side. As the ambient pressure is reduced, the jet column undergoes a series of spectacular transitions that are first marked by the appearance of vapor bubbles within the jet column. The transitions progress from columnar instabilities to series of column bifurcations to high-order branching and film formation and culminate in conical atomization of the jet column. In addition to the effects of the ambient pressure, the present investigation also considers effects of the liquid surface tension and vapor pressure on the onset, evolution, and hysteresis of the columnar transitions.

3-D matrix template-assisted growth of oriented oxide nanowire arrays using glancing angle pulsed laser deposition

NASA Astrophysics Data System (ADS)

Wright, N.; Mateo-Feliciano, D.; Ostoski, A.; Mukherjee, P.; Witanachchi, S.

Nanosphere lithography is a combination of different methods to nanofabrication. In this work nanosphere lithography is used to study the growth of Zinc Oxide Nano-columns (ZnO NCs) on different diameter Silica Nanosphere (SNS) self-assembled templates. ZnO NCs are promising building blocks for many existing and emerging optical, electrical, and piezoelectric devices, specifically, the seeded growth of other oxide materials. Recently, reports have shown a ferroelectric phase of zinc stannate (ZnSnO3) and while lead zirconium titanate oxide (PZT) has been the main material of interest in ferroelectric and piezoelectric applications, the toxicity of lead has been of great concern. The possibility of developing lead free piezoelectric materials is of great interest in the ferroelectric community. Langmuir-Blodgett method was used to construct a self-assembled monolayer of SNSs on silicon substrates. Oriented ZnO NCs were grown on top of the spheres using the glancing angle pulsed laser deposition technique. Columns were formed in a spatially ordered closed-packed hexagonal configuration. Growth of ZnO NCs was studied as function of ambient Oxygen pressure with SNS size ranging from 250-1000 nm. Cross-sectional Scanning Electron Microscopy and X-ray diffraction (XRD) were used to study the template structure. Relative aspect ratios were studied and showed tunability of column dimensions with sphere size. XRD revealed ZnO NC arrays were c-axis oriented with hexagonal wurtzite structure.

Electronics for fast ion extraction from EBIS devices

NASA Astrophysics Data System (ADS)

Höltermann, H.; Becker, R.; Kleinod, M.; Müller, I.

2004-05-01

Future synchrotrons for cancer therapy could profit from single turn injection in terms of size, costs, and ease of operation [O. Kester, R. Becker, and M. Kleinod, Rev. Sci. Instrum. 67 (1996)]. Short (˜1.5 μs) and intense (˜1.3 mA) pulses of highly charged light ions (C6+, N7+, O8+) are a requirement for these future therapy facilities which can be provided by an EBIS ion source. Such a medically dedicated EBIS has an electron beam of 400 mA at 5 keV and needs an electron current density of 100 A/cm2 for a repetition rate of 10 Hz. To obtain a 1.5 μs ion pulse it is necessary to switch the drift tube potentials up to 1.6 kV (for a ratio of beam to drift tube of 1/20) in some 100 ns. To avoid spreading out of the pulse due to the restoration of the full space charge depression at locations where ions have already been extracted, the potentials applied to the drift tubes are changed with time. They will be adjusted for each drift tube according to the transit time of the ion pulse. Furthermore, the drift tubes are fully interpenetrating each other with tapered fingers in order to locally distribute the action of the applied potentials. This provides a potential wall, which is following the extracted ion pulse and results in a compressed short ion pulse for single turn injection into a synchrotron.

Assessment of elemental mobility in soil using a fluidised bed approach with on-line ICP-MS analysis.

PubMed

Beeston, Michael Philip; Glass, Hylke Jan; van Elteren, Johannes Teun; Slejkovec, Zdenka

2007-09-19

A new method has been developed to analyse the mobility of elements within soils employing counter-current flow soil contacting in a fluidised bed (FB) column. This method alleviates the problem of irreproducible peaks suffered by state-of-the-art micro-column techniques as a result of particle compaction. Reproducible extraction profiles are produced through the leaching of soil with a linear gradient of 0.05 mol L(-1) ammonium sulphate to 0.11 mol L(-1) acetic acid using a high pressure liquid chromatography (HPLC) quaternary pump, and the continuous monitoring of the elements in the leachate with inductively coupled plasma mass spectrometry (ICP-MS). Quantification of the procedure is achieved with an external flow injection (FI) calibration method. Flow rate and FB column length were investigated as critical parameters to the efficiency of the extraction methodology. It was found that an increase in the column length from 10 to 20 cm using a flow rate of 0.15 mL min(-1) produced the same increase in extracted elemental concentration as an increase in flow rate from 0.15 to 0.30 mL min(-1). In both examples, the increase in the concentration of elements leached from the soil may be ascribed to the increase in the concentration gradient between the solid and liquid. The exhaustive nature of the technique defines the maximum leachable concentration within the operationally defined leaching parameters of the exchangeable phase, providing a more accurate assessment of the risk associated with the elements in the soil for the phase providing the greatest risk to the environment. The multi-elemental high sensitivity nature of the on-line detector provides an accurate determination of the associations present between the elements in the soil, and the identification of multiple phases within the exchangeable phase through the presence of multiple peaks in the extraction profiles. It is possible through the deconvolution of these extraction profiles that the concentration corresponding to the peaks identified can be defined.

5-O-caffeoylshikimic acid from Solanum somalense leaves: advantage of centrifugal partition chromatography over conventional column chromatography.

PubMed

Chideh, Saïda; Pilard, Serge; Attoumbré, Jacques; Saguez, Robert; Hassan-Abdallah, Alshaimaa; Cailleu, Dominique; Wadouachi, Anne; Baltora-Rosset, Sylvie

2014-09-01

Solanum somalense leaves, used in Djibouti for their medicinal properties, were extracted by MeOH. Because of the high polyphenol and flavonoid contents of the extract, respectively, determined at 80.80 ± 2.13 mg gallic acid equivalent/g dry weight and 24.4 ± 1.01 mg quercetin equivalent/g dry weight, the isolation and purification of the main polyphenols were carried out by silica gel column chromatography and centrifugal partition chromatography. Column chromatography led to 11 enriched fractions requiring further purification, while centrifugal partition chromatography allowed the easy recovery of the main compound of the extract. In a solvent system composed of CHCl3/MeOH/H2O (9.5:10:5), 21.8 mg of this compound at 97% purity was obtained leading to a yield of 2.63%. Its structure was established as 5-O-caffeoylshikimic acid by mass spectrometry and NMR spectroscopy. This work shows that S. somalense leaves contain very high level of 5-O-caffeoylshikimic acid (0.74% dry weight), making it a potential source of production of this secondary metabolite that is not commonly found in nature but could be partly responsible of the medicinal properties of S. somalense leaves. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Critical assessment of three high performance liquid chromatography analytical methods for food carotenoid quantification.

PubMed

Dias, M Graça; Oliveira, Luísa; Camões, M Filomena G F C; Nunes, Baltazar; Versloot, Pieter; Hulshof, Paul J M

2010-05-21

Three sets of extraction/saponification/HPLC conditions for food carotenoid quantification were technically and economically compared. Samples were analysed for carotenoids alpha-carotene, beta-carotene, beta-cryptoxanthin, lutein, lycopene, and zeaxanthin. All methods demonstrated good performance in the analysis of a composite food standard reference material for the analytes they are applicable to. Methods using two serial connected C(18) columns and a mobile phase based on acetonitrile, achieved a better carotenoid separation than the method using a mobile phase based on methanol and one C(18)-column. Carotenoids from leafy green vegetable matrices appeared to be better extracted with a mixture of methanol and tetrahydrofuran than with tetrahydrofuran alone. Costs of carotenoid determination in foods were lower for the method with mobile phase based on methanol. However for some food matrices and in the case of E-Z isomer separations, this was not technically satisfactory. Food extraction with methanol and tetrahydrofuran with direct evaporation of these solvents, and saponification (when needed) using pyrogallol as antioxidant, combined with a HPLC system using a slight gradient mobile phase based on acetonitrile and a stationary phase composed by two serial connected C(18) columns was the most technically and economically favourable method. 2010. Published by Elsevier B.V.

Optimising resolution for a preparative separation of Chinese herbal medicine using a surrogate model sample system.

PubMed

Ye, Haoyu; Ignatova, Svetlana; Peng, Aihua; Chen, Lijuan; Sutherland, Ian

2009-06-26

This paper builds on previous modelling research with short single layer columns to develop rapid methods for optimising high-performance counter-current chromatography at constant stationary phase retention. Benzyl alcohol and p-cresol are used as model compounds to rapidly optimise first flow and then rotational speed operating conditions at a preparative scale with long columns for a given phase system using a Dynamic Extractions Midi-DE centrifuge. The transfer to a high value extract such as the crude ethanol extract of Chinese herbal medicine Millettia pachycarpa Benth. is then demonstrated and validated using the same phase system. The results show that constant stationary phase modelling of flow and speed with long multilayer columns works well as a cheap, quick and effective method of optimising operating conditions for the chosen phase system-hexane-ethyl acetate-methanol-water (1:0.8:1:0.6, v/v). Optimum conditions for resolution were a flow of 20 ml/min and speed of 1200 rpm, but for throughput were 80 ml/min at the same speed. The results show that 80 ml/min gave the best throughputs for tephrosin (518 mg/h), pyranoisoflavone (47.2 mg/h) and dehydrodeguelin (10.4 mg/h), whereas for deguelin (100.5 mg/h), the best flow rate was 40 ml/min.

The transport and behaviour of isoproturon in unsaturated chalk cores

NASA Astrophysics Data System (ADS)

Besien, T. J.; Williams, R. J.; Johnson, A. C.

2000-04-01

A batch sorption study, a microcosm degradation study, and two separate column leaching studies were used to investigate the transport and fate of isoproturon in unsaturated chalk. The column leaching studies used undisturbed core material obtained from the field by dry percussion drilling. Each column leaching study used 25 cm long, 10 cm wide unsaturated chalk cores through which a pulse of isoproturon and bromide was eluted. The cores were set-up to simulate conditions in the unsaturated zone of the UK Chalk aquifer by applying a suction of 1 kPa (0.1 m H 2O) to the base of each column, and eluting at a rate corresponding to an average recharge rate through the unsaturated Chalk. A dye tracer indicated that the flow was through the matrix under these conditions. The results from the first column study showed high recovery rates for both isoproturon (73-92%) and bromide (93-96%), and that isoproturon was retarded by a factor of about 1.23 relative to bromide. In the second column study, two of the four columns were eluted with non-sterile groundwater in place of the sterile groundwater used on all other columns, and this study showed high recovery rates for bromide (85-92%) and lower recovery rates for isoproturon (66-79% — sterile groundwater, 48-61% — non-sterile groundwater). The enhanced degradation in the columns eluted with non-sterile groundwater indicated that groundwater microorganisms had increased the degradation rate within these columns. Overall, the reduced isoproturon recovery in the second column study was attributed to increased microbial degradation as a result of the longer study duration (162 vs. 105 days). The breakthrough curves (BTCs) for bromide had a characteristic convection-dispersion shape and were accurately simulated with the minimum of calibration using a simple convection-dispersion model (LEACHP). However, the isoproturon BTCs had an unusual shape and could not be accurately simulated.

Aluminum based metal-organic framework-polymer monolith in solid-phase microextraction of penicillins in river water and milk samples.

PubMed

Lirio, Stephen; Liu, Wan-Ling; Lin, Chen-Lan; Lin, Chia-Her; Huang, Hsi-Ya

2016-01-08

In this study, aluminum based metal-organic framework (Al-MOF)-organic polymer monoliths were prepared via microwave-assisted polymerization of ethylene dimethacrylate (EDMA), butyl methacrylate (BMA) with different weight percentages of Al-MOF (MIL-53; 37.5-62.5%) and subsequently utilized as sorbent in solid-phase microextraction (SPME) of penicillins (penicillin G, penicillin V, oxacillin, cloxacillin, dicloxacillin, nafcillin). The Al-MOF-polymer was characterized using Fourier transform infrared (FTIR) spectroscopy, powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and SEM-energy-dispersive X-ray spectroscopy (SEM-EDS) to clarify the retained crystalline structure well as the homogeneous dispersion of Al-MOF (MIL-53) in polymer monolith. The developed Al-MOF-polymer (MIL-53) monolithic column was evaluated according to its extraction recovery of penicillins. Several parameters affecting the extraction recoveries of penicillins using fabricated Al-MOF-polymer (MIL-53) monolithic column including different MIL-53 weight percentages, column length, pH, desorption solvent, and mobile phase flow rate were investigated. For comparison, different Al-based MOFs (MIL-68, CYCU-4 and DUT-5) were fabricated using the optimized condition for MIL-53-polymer (sample matrix at pH 3, 200μL desorption volume using methanol, 37.5% of MOF, 4-cm column length at 0.100mLmin(-1) flow rate). Among all the Al-MOF-polymers, MIL-53(Al)-polymer still afforded the best extraction recovery for penicillins ranging from 90.5 to 95.7% for intra-day with less than 3.5% relative standard deviations (RSDs) and inter-day precision were in the range of 90.7-97.6% with less than 4.2% RSDs. Meanwhile, the recoveries for column-to-column were in the range of 89.5-93.5% (<3.4% RSDs) while 88.5-90.5% (<5.8% RSDs) for batch-to-batch (n=3). Under the optimal conditions, the limit of detections were in the range of 0.06-0.26μgL(-1) and limit of quantifications between 0.20 and 0.87μgL(-1). Finally, the MIL-53-polymer was applied for the extraction of penicillin in river water and milk by spiking trace-level penicillin for as low as 50μgL(-1) and 100μgL(-1) with recoveries ranging from 80.8% to 90.9% (<6.7% RSDs) in river water and 81.1% to 100.7% (<7.1% RSDs) in milk sample, respectively. Copyright © 2015 Elsevier B.V. All rights reserved.

Pulsed counter-current ultrasound-assisted extraction and characterization of polysaccharides from Boletus edulis.

PubMed

You, Qinghong; Yin, Xiulian; Ji, Chaowen

2014-01-30

Four methods for extracting polysaccharides from Boletus edulis, namely, hot-water extraction, ultrasonic clearer extraction, static probe ultrasonic extraction, and pulsed counter-current probe ultrasonic extraction (CCPUE), were studied. Results showed that CCPUE has the highest extraction efficiency among the methods studied. Under optimal CCPUE conditions, a B. edulis polysaccharide (BEP) yield of 8.21% was obtained. Three purified fractions, BEP-I, BEP-II, and BEP-III, were obtained through sequential purification by DEAE-52 and Sephadex G-75 chromatography. The average molecular weights of BEP-I, BEP-II, and BEP-III were 10,278, 23,761, and 42,736 Da, respectively. The polysaccharides were mainly composed of xylose, mannose, galactose, and glucose; of these, mannose contents were the highest. The antioxidant activities of the BEPs were further investigated by measurement of their ability to scavenge DPPH and hydroxyl radicals as well as their reducing power. The results indicated that the BEPs have good antioxidant activity. Copyright © 2013 Elsevier Ltd. All rights reserved.

Effects of extraction and high-performance liquid chromatographic conditions on the determination of lutein in spinach.

PubMed

Simonovska, Breda; Vovk, Irena; Glavnik, Vesna; Cernelič, Katarina

2013-02-08

A major factor in the direct determination of lutein in spinach extracts proved to be obtaining reproducible and stable chromatography of lutein. This was achieved on a C30 column with the mobile phase acetone-0.1M triethylammonium acetate (TEAA) buffer (pH 7) 9:1 (v/v). Extraction of 10mg of lyophilized spinach with 10 mL of extraction solvent (ethanol, acetone, ethanol-ethyl acetate 1:1 (v/v), methanol-THF 1:1 (v/v)) for 15 min with magnetic stirring under nitrogen resulted in equal yields of lutein. The yields were enhanced by addition of 15% of 1M TEAA buffer pH 7 to all four extraction solvents. As confirmed by recovery experiments, no loss of lutein occurred during the extraction. The relative standard deviation from triplicate extractions was less than 5%. The addition of 15% TEAA pH 7 to acetone enhanced the extraction yield of lutein also from unlyophilized spinach. The content of lutein in different spinach samples ranged from 5 to 15 mg/100g of fresh weight. The first separation is reported of all the carotenoids and chlorophylls on a C18 core-shell column and the addition of 15% of 1M TEAA buffer pH 7 to acetone also enhanced the extraction yield of β-carotene compared to the yield produced by pure acetone. Copyright © 2012 Elsevier B.V. All rights reserved.

Home-made online hyphenation of pressurized liquid extraction, turbulent flow chromatography, and high performance liquid chromatography, Cistanche deserticola as a case study.

PubMed

Song, Qingqing; Li, Jun; Liu, Xiao; Zhang, Yuan; Guo, Liping; Jiang, Yong; Song, Yuelin; Tu, Pengfei

2016-03-18

Incompatibility between the conventional pressurized liquid extraction (PLE) devices and high performance liquid chromatography (HPLC) extensively hinders direct and green chemical analysis of herbal materials. Herein, a facile PLE module was configured, and then it was online hyphenated with HPLC via a turbulent flow chromatography (TFC) column. Regarding PLE module, a long PEEK tube (0.13 × 1000 mm) was employed to generate desired pressure (approximately 13.0 MPa) when warm acidic water (70 °C) was delivered as extraction solvent at a high flow rate (2.5 mL/min), and a hollow guard column (3.0 × 4.0 mm) was implemented to hold crude materials. Effluent was collected from the outlet of PEEK tube, concentrated, and subjected onto HPLC coupled with hybrid ion trap-time of flight mass spectrometer to assess the extraction efficiency and also to profile the chemical composition of Cistanche deserticola (CD) that is honored as "Ginseng of the desert". Afterwards, a TFC column was introduced to accomplish online transmission of low molecule weight components from PLE module to HPLC coupled with diode array detection, and two electronic 6-port/2-channel valves were in charge of alternating the whole system between extraction (0-3.0 min) and elution (3.0-35.0 min) phases. Quantitative method was developed and validated for simultaneous determination of eight primary phenylethanoid glycosides in CD using online PLE-TFC-HPLC. All findings demonstrated that the home-made platform is advantageous at direct chemical analysis, as well as time-, solvent-, and material-savings, suggesting a robust tool for chemical fingerprinting of herbs. Copyright © 2016 Elsevier B.V. All rights reserved.

High efficiency liquid chromatography techniques coupled to mass spectrometry for the characterization of mate extracts.

PubMed

Dugo, Paola; Cacciola, Francesco; Donato, Paola; Jacques, Rosângela Assis; Caramão, Elina Bastos; Mondello, Luigi

2009-10-23

There is growing interest related to rapid screening and full characterization of the constituents of plants with medicinal properties; among these, "Mate" or Yerba Maté is a tea-like beverage widely consumed in South America, obtained from the dried leaves of Ilex paraguariensis. The high content in polyphenols accounts for in vitro and in vivo antioxidant activity of the extracts obtained from this plant; on the other hand, the high complexity of the samples extracted, depending on the method employed, may preclude complete resolution by conventional HPLC techniques. For this purpose, a comprehensive two-dimensional liquid chromatography (LC x LC) system, comprised of an RP-Amide first dimension and a partially porous octadecylsilica column in the second dimension, has been compared with a one-dimensional system. The latter was operated using a partially porous octadecylsilica column, with diode array (DAD) and electrospray/ion trap-time of flight (ESI/IT-TOF) detection for the most complex extracts. The employment of the hybrid mass spectrometer allowed unequivocal identification of several compounds in the mate extracts. Using LC x LC-MS(3), it was possible to discriminate between congeners of chlorogenic acids, along with monoacyl- and diacylchlorogenic acid esters.

Method of analysis and quality-assurance practices for determination of pesticides in water by solid-phase extraction and capillary-column gas chromatography/mass spectrometry at the U.S. Geological Survey California District Organic Chemistry Laboratory, 1996-99

USGS Publications Warehouse

Crepeau, Kathryn L.; Baker, Lucian M.; Kuivila, Kathryn

2000-01-01

A method of analysis and quality-assurance practices were developed to study the fate and transport of pesticides in the San Francisco Bay-Estuary by the U.S. Geological Survey. Water samples were filtered to remove suspended-particulate matter and pumped through C-8 solid-phase extraction cartridges to extract the pesticides. The cartridges were dried with carbon dioxide and the pesticides were eluted with three cartridge volumes of hexane:diethyl ether (1:1) solution. The eluants were analyzed using capillary-column gas chromatography/mass spectrometry in full-scan mode. Method detection limits for pesticides ranged from 0.002 to 0.025 microgram per liter for 1-liter samples. Recoveries ranged from 44 to 140 percent for 25 pesticides in samples of organic-free reagent water and Sacramento-San Joaquin Delta and Suisun Bay water fortified at 0.05 and 0.50 microgram per liter. The estimated holding time for pesticides after extraction on C-8 solid-phase extraction cartridges ranged from 10 to 257 days.

Intense laser pulse propagation in capillary discharge plasma channels

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

Hubbard, R.F.; Moore, C.I.; Sprangle, P.

Optical guiding of intense laser pulses is required for plasma-based accelerator concepts such as the laser wakefield accelerator. Reported experiments have successfully transported intense laser pulses in the hollow plasma column produced by a capillary discharge. The hollow plasma has an index of refraction which peaks on-axis, thus providing optical guiding which overcomes beam expansion due to diffraction. In more recent experiments at Hebrew University, 800 nm wavelength, 0.1 mJ, 100 fs pulses have been guided in {approximately}300 micron radius capillaries over distances as long as 6.6 cm. Simulations of these experiments using a 2-D nonlinear laser propagation model producemore » the expected optical guiding, with the laser pulse radius r{sub L} exhibiting oscillations about the equilibrium value predicted by an analytical envelope equation model. The oscillations are damped at the front of the pulse and grow in amplitude in the back of the pulse. This growth and damping is attributed to finite pulse length effects. Simulations also show that further ionization of the discharge plasma by the laser pulse may hollow the laser pulse and introduce modulations in the spot size. This ionization-defocusing effect is expected to be significant at the high intensities required for accelerator application. Capillary discharge experiments at much higher intensities are in progress on the Naval Research Laboratory T{sup 3} laser, and preliminary results are reported. {copyright} {ital 1999 American Institute of Physics.}« less

The effect of re-dissolution solvents and HPLC columns on the analysis of mycosporine-like amino acids in the eulittoral macroalgae Prasiola crispa and Porphyra umbilicalis

NASA Astrophysics Data System (ADS)

Karsten, Ulf; Escoubeyrou, Karine; Charles, François

2009-09-01

Many macroalgal species that are regularly exposed to high solar radiation such as the eulittoral green alga Prasiola crispa and the red alga Porphyra umbilicalis synthesize and accumulate high concentrations of mycosporine-like amino acids (MAAs) as UV-sunscreen compounds. These substances are typically extracted with a widely used standard protocol following quantification by various high performance liquid chromatography (HPLC) techniques. However, further preparation steps prior to HPLC analysis as well as different HPLC column types have not been systematically checked regarding separation quality and reproducibility. Therefore pure methanol, distilled water and HPLC eluent were evaluated as re-dissolution solvent for dried Prasiola and Porphyra extracts, which were subsequently analyzed on three reversed-phase C8 and C18 HPLC columns. The data indicate that distilled water and the HPLC eluent gave almost identical peak patterns and MAA contents on the C8 and C18 columns. In contrast, the application of the widely used methanol led to double peaks or even the loss of specific peaks as well as to a strong decline in total MAA amounts ranging from about 35% of the maximum in P. crispa to 80% of the maximum in P. umbilicalis. Consequently, methanol should be avoided as re-dissolution solvent for the HPLC sample preparation. An improved protocol for the MAA analysis in macroalgae in combination with a reliable C18 column is suggested.

Ion chromatographic methods for the detection of starch hydrolysis products in ruminal digesta.

PubMed

Barsuhn, K; Kotarski, S F

1991-06-21

Dionex high-performance ion chromatographic methods were evaluated for separation and quantitation of plant sugars and starch digestion products in the ruminal digesta of cattle. Mono- and disaccharides were eluted from a Dionex CarboPac PA1 column with sodium hydroxide used isocratically or as a pH gradient. Maltooligosaccharides which had a degree of polymerization (DP) less than 30 glucose residues were eluted in 60 min by a sodium hydroxide eluent containing a sodium acetate gradient. Carbohydrates were detected amperometrically. Responses were linear (r2 greater than 0.99) for glucose, disaccharides and maltooligosaccharides (DP less than 8). Precipitation and solid-phase extraction methods were evaluated for clean-up of samples of feedstuffs, ruminal contents, and bacterial culture fluids. Perchloric acid precipitation hydrolyzed sucrose but did not affect recoveries of cellobiose, isomaltose or maltose. Ethanol in concentrations of 79 and 86% precipitated maltooligosaccharides having chain lengths larger than 14 and 9 glucose residues, respectively. Maltooligosaccharide recoveries from solid-phase extraction columns varied with maltooligosaccharide size and column packing. Recoveries were greater than 94% for short chains (DP less than 6) eluted from phenyl-substituted columns and variable for all oligosaccharides eluted from C18 columns. Applications of these methods are presented and include: (1) detection of sugars in ruminant feed, (2) monitoring changes in ruminal sugars after feeding and (3) monitoring changes in extracellular sugars and oligosaccharides in the culture fluids of the ruminal bacterium, Bacteroides ruminicola.

Analysis of underivatised low volatility compounds by comprehensive two-dimensional gas chromatography with a short primary column.

PubMed

Novaes, Fábio Junior Moreira; Kulsing, Chadin; Bizzo, Humberto Ribeiro; de Aquino Neto, Francisco Radler; Rezende, Claudia Moraes; Marriott, Philip John

2018-02-09

Comprehensive two-dimensional gas chromatography (GC×GC) approaches with cryogenic modulation were developed for the qualitative analysis of selected low volatility compounds in raw coffee bean extracts, without derivatisation. The approaches employed short first ( 1 D) and second ( 2 D) dimension columns, specifically a 1 D 65% phenyl methyl siloxane column (11m) and a 2 D 5% phenyl methyl siloxane column (1m), which allowed elution of high molar mass compounds (e.g.>600Da). Solutes included hydrocarbons, fatty acids, diterpenes, tocopherols, sterols, diterpene esters, and di- and triacylglycerides. An oven temperature program up to 370°C was employed. The effects of experimental conditions were investigated, revealing that the GC×GC results strongly depended on the cryogenic trap T, and oven T program. An appropriate condition was selected and further applied for group type analysis of low volatility compounds in green Arabica coffee beans. Retention indices were compiled for 1D GC analysis and were similar for the composite column data in GC×GC. The elution of some compounds was confirmed by use of authentic standards. The approach allowed direct analysis of coffee extract in ethyl acetate solution, with improved analyte peak capacity (approximately 200 compounds were detected) without prior fractionation or pre-treatment of the sample. This avoided potential hydrolysis of high molar mass conjugate esters as well as degradation of thermally labile compounds such as the derivatives of the diterpenes cafestol and kahweol. Copyright © 2017 Elsevier B.V. All rights reserved.

Binary solvent extraction system and extraction time effects on phenolic antioxidants from kenaf seeds (Hibiscus cannabinus L.) extracted by a pulsed ultrasonic-assisted extraction.

PubMed

Wong, Yu Hua; Lau, Hwee Wen; Tan, Chin Ping; Long, Kamariah; Nyam, Kar Lin

2014-01-01

The aim of this study was to determine the best parameter for extracting phenolic-enriched kenaf (Hibiscus cannabinus L.) seeds by a pulsed ultrasonic-assisted extraction. The antioxidant activities of ultrasonic-assisted kenaf seed extracts (KSE) were determined by a 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging capacity assay, 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid) (ABTS) radical scavenging assay, β -carotene bleaching inhibition assay, and ferric reducing antioxidant power (FRAP) assay. Total phenolic content (TPC) and total flavonoid content (TFC) evaluations were carried out to determine the phenolic and flavonoid contents in KSE. The KSE from the best extraction parameter was then subjected to high performance liquid chromatography (HPLC) to quantify the phenolic compounds. The optimised extraction condition employed 80% ethanol for 15 min, with the highest values determined for the DPPH, ABTS, and FRAP assay. KSE contained mainly tannic acid (2302.20 mg/100 g extract) and sinapic acid (1198.22 mg/100 g extract), which can be used as alternative antioxidants in the food industry.

Binary Solvent Extraction System and Extraction Time Effects on Phenolic Antioxidants from Kenaf Seeds (Hibiscus cannabinus L.) Extracted by a Pulsed Ultrasonic-Assisted Extraction

PubMed Central

Lau, Hwee Wen; Nyam, Kar Lin

2014-01-01

The aim of this study was to determine the best parameter for extracting phenolic-enriched kenaf (Hibiscus cannabinus L.) seeds by a pulsed ultrasonic-assisted extraction. The antioxidant activities of ultrasonic-assisted kenaf seed extracts (KSE) were determined by a 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging capacity assay, 2,2′-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid) (ABTS) radical scavenging assay, β-carotene bleaching inhibition assay, and ferric reducing antioxidant power (FRAP) assay. Total phenolic content (TPC) and total flavonoid content (TFC) evaluations were carried out to determine the phenolic and flavonoid contents in KSE. The KSE from the best extraction parameter was then subjected to high performance liquid chromatography (HPLC) to quantify the phenolic compounds. The optimised extraction condition employed 80% ethanol for 15 min, with the highest values determined for the DPPH, ABTS, and FRAP assay. KSE contained mainly tannic acid (2302.20 mg/100 g extract) and sinapic acid (1198.22 mg/100 g extract), which can be used as alternative antioxidants in the food industry. PMID:24592184

An updated ciguatoxin extraction method and silica cleanup for use with HPLC-MS/MS for the analysis of P-CTX-1, PCTX-2 and P-CTX-3.

PubMed

Meyer, Lauren; Carter, Steve; Capper, Angela

2015-12-15

Ciguatera fish poisoning is a debilitating human neuro-intoxication caused by consumption of tropical marine organisms, contaminated with bioaccumulated ciguatoxins (CTXs). The growing number of cases coupled with the high toxicity of CTXs makes their reliable detection and quantification of paramount importance. Three commonly occurring ciguatoxins, P-CTX-1, 2 and 3 from five different ciguatoxic Spanish mackerel (Scomberomorus commerson), were used to assess the effectiveness of different extraction techniques: homogenization (high powered blending vs. ultrasonication); C-18 column sizes (500 mg vs. 900 mg); and a novel HILIC SPE cleanup. Despite minor differences, blending and sonication proved equally effective. Larger 900 mg columns offered a greater extraction efficiency, increasing detected P-CTX-1 by 37% (P < 0.001). The newly adapted cleanup was highly effective at reducing co-eluting phospholipids thereby reducing matrix effects and increasing detectable CTXs by HPLC-MS/MS. Silica cleanup extraction efficiencies were also compared between the highly effective and validated ciguatoxin rapid extraction method (CREM) and current best practice extraction method employed by Queensland Health (QH). Overall, the QH protocol proved more effective, especially when paired with the newly adapted cleanup, as this increased the amount of extracted P-CTX-1 by 46% (P < 0.01), P-CTX-2 by 10% and P-CTX-3 by 71% (P = 0.001). This study suggests the QH protocol utilizing a 900 mg C-18 column and newly adapted HILIC SPE cleanup was most effective at extracting P-CTX-1, -2, -3. Specifically P-CTX-1, the primary ciguatoxin congener of concern due to its extremely high potency and an ability to cause CFP at 0.1 μg/kg following consumption of carnivorous fish flesh. Despite being more time intensive (an additional 85 min per batch of 12 samples), this will be especially effective for assessing lower toxin burdens, which may be near the limit of detection. Copyright © 2015 Elsevier Ltd. All rights reserved.

On-line hyphenation of solid-phase extraction to chromatographic separation of sulfonamides with fused-core columns in sequential injection chromatography.

PubMed

Batista, Alex D; Chocholouš, Petr; Satínský, Dalibor; Solich, Petr; Rocha, Fábio R P

2015-02-01

On-line sample pretreatment (clean-up and analyte preconcentration) is for the first time coupled to sequential injection chromatography. The approach combines anion-exchange solid-phase extraction and the highly effective pentafluorophenylpropyl (F5) fused-core particle column for separation of eight sulfonamide antibiotics with similar structures (sulfathiazole, sulfanilamide, sulfacetamide, sulfadiazine, sulfamerazine, sulfadimidine, sulfamethoxazole and sulfadimethoxine). The stationary phase was selected after a critical comparison of the performance achieved by three fused-core reversed phase columns (Ascentis(®) Express RP-Amide, Phenyl-Hexyl, and F5) and two monolithic columns (Chromolith(®) High Resolution RP-18 and CN). Acetonitrile and acetate buffer pH 5.0 at 0.60 mL min(-1) were used as mobile phase to perform the separations before spectrophotometric detection. The first mobile phase was successfully used as eluent from SPE column ensuring transfer of a narrow zone to the chromatographic column. Enrichment factors up to 39.2 were achieved with a 500 µL sample volume. The developed procedure showed analysis time <10.5 min, resolutions >1.83 with peak symmetry ≤1.52, LODs between 4.9 and 27 µg L(-1), linear response ranges from 30.0 to 1000.0 µg L(-1) (r(2)>0.996) and RSDs of peak heights <2.9% (n=6) at a 100 µg L(-1) level and enabled the screening control of freshwater samples contaminated at the 100 µg L(-1) level. The proposed approach expanded the analytical potentiality of SIC and avoided the time-consuming batch sample pretreatment step, thus minimizing risks of sample contamination and analyte losses. Copyright © 2014 Elsevier B.V. All rights reserved.

Airborne Measurements of CO2 Column Concentration and Range Using a Pulsed Direct-Detection IPDA Lidar

NASA Technical Reports Server (NTRS)

Abshire, James B.; Ramanathan, Anand; Riris, Haris; Mao, Jianping; Allan, Graham R.; Hasselbrack, William E.; Weaver, Clark J.; Browell, Edward V.

2013-01-01

We have previously demonstrated a pulsed direct detection IPDA lidar to measure range and the column concentration of atmospheric CO2. The lidar measures the atmospheric backscatter profiles and samples the shape of the 1,572.33 nm CO2 absorption line. We participated in the ASCENDS science flights on the NASA DC-8 aircraft during August 2011 and report here lidar measurements made on four flights over a variety of surface and cloud conditions near the US. These included over a stratus cloud deck over the Pacific Ocean, to a dry lake bed surrounded by mountains in Nevada, to a desert area with a coal-fired power plant, and from the Rocky Mountains to Iowa, with segments with both cumulus and cirrus clouds. Most flights were to altitudes >12 km and had 5-6 altitude steps. Analyses show the retrievals of lidar range, CO2 column absorption, and CO2 mixing ratio worked well when measuring over topography with rapidly changing height and reflectivity, through thin clouds, between cumulus clouds, and to stratus cloud tops. The retrievals shows the decrease in column CO2 due to growing vegetation when flying over Iowa cropland as well as a sudden increase in CO2 concentration near a coal-fired power plant. For regions where the CO2 concentration was relatively constant, the measured CO2 absorption lineshape (averaged for 50 s) matched the predicted shapes to better than 1% RMS error. For 10 s averaging, the scatter in the retrievals was typically 2-3 ppm and was limited by the received signal photon count. Retrievals were made using atmospheric parameters from both an atmospheric model and from in situ temperature and pressure from the aircraft. The retrievals had no free parameters and did not use empirical adjustments, and >70% of the measurements passed screening and were used in analysis. The differences between the lidar-measured retrievals and in situ measured average CO2 column concentrations were <1.4 ppm for flight measurement altitudes >6 km.

Biodegradation of the surfactant linear alkylbenzenesulfonate in sewage- contaminated groundwater: A comparison of column experiments and field tracer tests

USGS Publications Warehouse

Krueger, C.J.; Radakovich, K.M.; Sawyer, T.E.; Barber, L.B.; Smith, R.L.; Field, J.A.

1998-01-01

Transport and biodegradation of linear alkylbenzenesulfonate (LAS) in sewage-contaminated groundwater were investigated for a range of dissolved oxygen concentrations. Both laboratory column and an 80-day continuous injection tracer test field experiments were conducted. The rates of LAS biodegradation increased with increasing dissolved oxygen concentrations and indicated the preferential biodegradation of the longer alkyl chain LAS homologues (i.e., C12 and C13) and external isomers (i.e., 2-and 3- phenyl). However, for similar dissolved oxygen concentrations, mass removal rates for LAS generally were 2-3 times greater in laboratory column experiments than in the field tracer test. Under low oxygen conditions (<1 mg/L) only a fraction of the LAS mixture biodegraded in both laboratory and field experiments. Biodegradation rate constants for the continuous injection field test (0.002-0.08 day-1) were comparable to those estimated for a 3-h injection (pulsed) tracer test conducted under similar biogeochemical conditions, indicating that increasing the exposure time of aquifer sediments to LAS did not increase biodegradation rates.Transport and biodegradation of linear alkylbenzenesulfonate (LAS) in sewage-contaminated groundwater were investigated for a range of dissolved oxygen concentrations. Both laboratory column and an 80-day continuous injection tracer test field experiments were conducted. The rates of LAS biodegradation increased with increasing dissolved oxygen concentrations and indicated the preferential biodegradation of the longer alkyl chain LAS homologues (i.e., C12 and C13) and external isomers (i.e., 2- and 3-phenyl). However, for similar dissolved oxygen concentrations, mass removal rates for LAS generally were 2-3 times greater in laboratory column experiments than in the field tracer test. Under low oxygen conditions (<1 mg/L) only a fraction of the LAS mixture biodegraded in both laboratory and field experiments. Biodegradation rate constants for the continuous injection field test (0.002-0.08 day-1) were comparable to those estimated for a 3-h injection (pulsed) tracer test conducted under similar biogeochemical conditions, indicating that increasing the exposure time of aquifer sediments to LAS did not increase biodegradation rates.

Production of the biopesticide azadirachtin by hairy root cultivation of Azadirachta indica in liquid-phase bioreactors.

PubMed

Srivastava, Smita; Srivastava, Ashok K

2013-11-01

Batch cultivation of Azadirachta indica hairy roots was carried out in different liquid-phase bioreactor configurations (stirred-tank, bubble column, bubble column with polypropylene basket, and polyurethane foam disc as root supports) to investigate possible scale-up of the A. indica hairy root culture for in vitro production of the biopesticide azadirachtin. The hairy roots failed to grow in the conventional bioreactor designs (stirred tank and bubble column). However, modified bubble column reactor (with polyurethane foam as root support) configuration facilitated high-density culture of A. indica hairy roots with a biomass production of 9.2 g l(-1)dry weight and azadirachtin yield of 3.2 mg g(-1) leading to a volumetric productivity of azadirachtin as 1.14 mg l(-1) day(-1). The antifeedant activity in the hairy roots was also evaluated by no choice feeding tests with known concentrations of the hairy root powder and its solvent extract separately on the desert locust Schistocerca gregaria. The hairy root powder and its solvent extract demonstrated a high level of antifeedant activity (with an antifeedant index of 97 % at a concentration of 2 % w/v and 83 % at a concentration of 0.05 % (w/v), respectively, in ethanol).

A strategy for identification and structural characterization of compounds from Gardenia jasminoides by integrating macroporous resin column chromatography and liquid chromatography-tandem mass spectrometry combined with ion-mobility spectrometry.

PubMed

Wang, Lu; Liu, Shu; Zhang, Xueju; Xing, Junpeng; Liu, Zhiqiang; Song, Fengrui

2016-06-24

In this paper, an analysis strategy integrating macroporous resin (AB-8) column chromatography and high performance liquid chromatography-electrospray ionization-tandem mass spectrometry (HPLC-ESI-MS/MS) combined with ion mobility spectrometry (IMS) was proposed and applied for identification and structural characterization of compounds from the fruits of Gardenia jasminoides. The extracts of G. jasminoides were separated by AB-8 resin column chromatography combined with reversed phase liquid chromatography (C18 column) and detected by electrospray ionization tandem mass spectrometry. Additionally, ion mobility spectrometry (IMS) was employed as a supplementary separation technique to discover previously undetected isomers from the fruits of G. jasminoides. A total of 71 compounds, including iridoids, flavonoids, triterpenes, monoterpenoids, carotenoids and phenolic acids were identified by the characteristic high resolution mass spectrometry and the ESI-MS/MS fragmentations. In conclusion, the IMS-MS technique achieved the separation of isomers in crocin-3 and crocin-4 according to their acquired mobility drift times differing from classical analysis by mass spectrometry. The proposed strategy can be used as a highly sensitive and efficient procedure for identification and separation isomeric components in extracts of herbal medicines. Copyright © 2016 Elsevier B.V. All rights reserved.

The perils of pathogen discovery: origin of a novel parvovirus-like hybrid genome traced to nucleic acid extraction spin columns.

PubMed

Naccache, Samia N; Greninger, Alexander L; Lee, Deanna; Coffey, Lark L; Phan, Tung; Rein-Weston, Annie; Aronsohn, Andrew; Hackett, John; Delwart, Eric L; Chiu, Charles Y

2013-11-01

Next-generation sequencing was used for discovery and de novo assembly of a novel, highly divergent DNA virus at the interface between the Parvoviridae and Circoviridae. The virus, provisionally named parvovirus-like hybrid virus (PHV), is nearly identical by sequence to another DNA virus, NIH-CQV, previously detected in Chinese patients with seronegative (non-A-E) hepatitis. Although we initially detected PHV in a wide range of clinical samples, with all strains sharing ∼99% nucleotide and amino acid identity with each other and with NIH-CQV, the exact origin of the virus was eventually traced to contaminated silica-binding spin columns used for nucleic acid extraction. Definitive confirmation of the origin of PHV, and presumably NIH-CQV, was obtained by in-depth analyses of water eluted through contaminated spin columns. Analysis of environmental metagenome libraries detected PHV sequences in coastal marine waters of North America, suggesting that a potential association between PHV and diatoms (algae) that generate the silica matrix used in the spin columns may have resulted in inadvertent viral contamination during manufacture. The confirmation of PHV/NIH-CQV as laboratory reagent contaminants and not bona fide infectious agents of humans underscores the rigorous approach needed to establish the validity of new viral genomes discovered by next-generation sequencing.

A rapid silica spin column-based method of RNA extraction from fruit trees for RT-PCR detection of viruses.

PubMed

Yang, Fan; Wang, Guoping; Xu, Wenxing; Hong, Ni

2017-09-01

Efficient recovery of high quality RNA is very important for successful RT-PCR detection of plant RNA viruses. High levels of polyphenols and polysaccharides in plant tissues can irreversibly bind to and/or co-precipitate with RNA, which influences RNA isolation. In this study, a silica spin column-based RNA isolation method was developed by using commercially available silica columns combined with the application of a tissue lysis solution, and binding and washing buffers with high concentration guanidinium thiocyanate (GuSCN, 50% w/v), which helps remove plant proteins, polysaccharides and polyphenolic compounds. The method was successfully used to extract high quality RNA from citrus (Citrus aurantifolia), grapevine (Vitis vinifera), peach (Prunus persica), pear (Pyrus spp.), taro (Colocosia esculenta) and tobacco (Nicotiana benthamiana) samples. The method was comparable to conventional CTAB method in RNA isolation efficiency, but it was more sample-adaptable and cost-effective than commercial kits. High quality RNA isolated using silica spin column-based method was successfully used for the RT-PCR and/or multiplex RT-PCR amplification of woody fruit tree viruses and a viroid. The study provided a useful tool for the detection and characterization of plant viruses. Copyright © 2017 Elsevier B.V. All rights reserved.

Comprehensive two-dimensional HPLC to study the interaction of multiple components in Rheum palmatum L. with HSA by coupling a silica-bonded HSA column to a silica monolithic ODS column.

PubMed

Hu, Lianghai; Li, Xin; Feng, Shun; Kong, Liang; Su, Xingye; Chen, Xueguo; Qin, Feng; Ye, Mingliang; Zou, Hanfa

2006-04-01

A mode of comprehensive 2-D LC was developed by coupling a silica-bonded HSA column to a silica monolithic ODS column. This system combined the affinity property of the HSA column and the high-speed separation ability of the monolithic ODS column. The affinity chromatography with HSA-immobilized stationary phase was applied to study the interaction of multiple components in traditional Chinese medicines (TCMs) with HSA according to their affinity to protein in the first dimension. Then the unresolved components retained on the HSA column were further separated on the silica monolithic ODS column in the second dimension. By hyphenating the 2-D separation system to diode array detector and MS detectors, the UV and molecular weight information of the separated compounds can also be obtained. The developed separation system was applied to analysis of the extract of Rheum palmatum L., a number of low-abundant components can be separated on a single peak from the HSA column after normalization of peak heights. Six compounds were preliminarily identified according to their UV and MS spectra. It showed that this system was very useful for biological fingerprinting analysis of the components in TCMs and natural products.

Ultra-Trace Analysis of Nine Macrolides, including Tulathromycin A (Draxxin), in Edible Animal Tissues with Mini-Column Liquid Chromatography Tandem Mass Spectrometry

USDA-ARS?s Scientific Manuscript database

Analysis of 9 macrolides is presented, including tulathromycin A (Draxxin), in beef, poultry and pork muscle with a simple multi-residue extraction and analysis method using high performance liquid chromatography coupled to electrospray ionization tandem mass spectrometry. The extraction method inv...

EPA Method 525.3 - Determination of Semivolatile Organic Chemicals in Drinking Water by Solid Phase Extraction and Capillary Column Gas Chromatography/Mass Spectrometry (GC/MS)

EPA Science Inventory

Method 525.3 is an analytical method that uses solid phase extraction (SPE) and gas chromatography/mass spectrometry (GC/MS) for the identification and quantitation of 125 selected semi-volatile organic chemicals in drinking water.

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

Blay, J.A.

The problem of the determination of micro-amounts of uranium in aqueous and organic phases in liquid-liquid extraction processes, original ones, and extraction residues was solved by a chromatographic separation of the uranium by means of columns of activated cellulose and further spectrophotometric evaluation using the thiocyanate complex in aqueous medium. The usable range is 5 to 200 mu g.

Simplified multiple headspace extraction gas chromatographic technique for determination of monomer solubility in water.

PubMed

Chai, X S; Schork, F J; DeCinque, Anthony

2005-04-08

This paper reports an improved headspace gas chromatographic (GC) technique for determination of monomer solubilities in water. The method is based on a multiple headspace extraction GC technique developed previously [X.S. Chai, Q.X. Hou, F.J. Schork, J. Appl. Polym. Sci., in press], but with the major modification in the method calibration technique. As a result, only a few iterations of headspace extraction and GC measurement are required, which avoids the "exhaustive" headspace extraction, and thus the experimental time for each analysis. For highly insoluble monomers, effort must be made to minimize adsorption in the headspace sampling channel, transportation conduit and capillary column by using higher operating temperature and a short capillary column in the headspace sampler and GC system. For highly water soluble monomers, a new calibration method is proposed. The combinations of these technique modifications results in a method that is simple, rapid and automated. While the current focus of the authors is on the determination of monomer solubility in aqueous solutions, the method should be applicable to determination of solubility of any organic in water.

Toxicity of plant extracts containing pyrrolizidine alkaloids using alternative invertebrate models.

PubMed

Seremet, Oana Cristina; Olaru, Octavian Tudorel; Gutu, Claudia Maria; Nitulescu, George Mihai; Ilie, Mihaela; Negres, Simona; Zbarcea, Cristina Elena; Purdel, Carmen Nicoleta; Spandidos, Demetrios A; Tsatsakis, Aristides M; Coleman, Michael D; Margina, Denisa Marilena

2018-06-01

Pyrrolizidine alkaloids (PAs) are a widespread class of hepatotoxic heterocyclic organic compounds found in approximately 3% of world flora. Some PAs have been shown to have genotoxic and carcinogenic effects. The present study focuses on the toxicity effects of four dry extracts obtained from medicinal plants (Senecio vernalis, Symphytum officinale, Petasites hybridus and Tussilago farfara), on two aquatic organisms, Artemia salina and Daphnia magna, and the correlation with their PAs content. A new GC‑MS method, using a retention time (TR)‑5MS type capillary column was developed. PAs Kovats retention indices, for this type of column were computed for the first time. The lethal dose 50% (LC50) values for the two invertebrate models were correlated (Pearson 's coefficient, >0.9) and the toxicity was PA concentration-dependent, for three of the four extracts. All tested extracts were found to be toxic in both aquatic organism models. The results can be used to develop a GC‑MS validated method for the assay of PAs in medicinal plants with a further potential application in the risk assessment study of PAs toxicity in humans.

Toxicity of plant extracts containing pyrrolizidine alkaloids using alternative invertebrate models

PubMed Central

Seremet, Oana Cristina; Olaru, Octavian Tudorel; Gutu, Claudia Maria; Nitulescu, George Mihai; Ilie, Mihaela; Negres, Simona; Zbarcea, Cristina Elena; Purdel, Carmen Nicoleta; Spandidos, Demetrios A.; Tsatsakis, Aristides M.; Coleman, Michael D.; Margina, Denisa Marilena

2018-01-01

Pyrrolizidine alkaloids (PAs) are a widespread class of hepatotoxic heterocyclic organic compounds found in approximately 3% of world flora. Some PAs have been shown to have genotoxic and carcinogenic effects. The present study focuses on the toxicity effects of four dry extracts obtained from medicinal plants (Senecio vernalis, Symphytum officinale, Petasites hybridus and Tussilago farfara), on two aquatic organisms, Artemia salina and Daphnia magna, and the correlation with their PAs content. A new GC-MS method, using a retention time (TR)-5MS type capillary column was developed. PAs Kovats retention indices, for this type of column were computed for the first time. The lethal dose 50% (LC50) values for the two invertebrate models were correlated (Pearson's coefficient, >0.9) and the toxicity was PA concentration-dependent, for three of the four extracts. All tested extracts were found to be toxic in both aquatic organism models. The results can be used to develop a GC-MS validated method for the assay of PAs in medicinal plants with a further potential application in the risk assessment study of PAs toxicity in humans. PMID:29620235

Plasma expansion into a waveguide created by a linearly polarized femtosecond laser pulse

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

Lemos, N.; Grismayer, T.; Cardoso, L.

2013-06-15

We demonstrate the efficient generation of 4 mm and 8 mm long plasma waveguides in hydrogen and helium. These waveguides have matching spots sizes for 13 to 34 μm laser beams. The plasma waveguides are created by ultra-short laser pulses (sub-picosecond) of moderate intensities, ∼10{sup 15}–10{sup 16} W cm{sup −2}, that heat the plasma to initial temperatures of tens of eV in order to create a hot plasma column that will expand into a plasma waveguide. We have determined that the main heating mechanism when using fs laser pulses and plasma densities ∼10{sup 18–19} cm{sup −3} is Above Threshold Ionization.more » Detailed time and space electron density measurements are presented for the laser produced plasma waveguides.« less

A Novel Triple-Pulsed 2-micrometer Lidar for Simultaneous and Independent CO2 and H2O Column Measurement

NASA Technical Reports Server (NTRS)

Yu, Jirong; Singh, Upendra; Petros, Mulugeta; Refaat, Tamer

2015-01-01

The study of global warming needs precisely and accurately measuring greenhouse gases concentrations in the atmosphere. CO2 and H2O are important greenhouse gases that significantly contribute to the carbon cycle and global radiation budget on Earth. NRC Decadal Survey recommends a mission for Active Sensing of Carbon Dioxide (CO2) over Nights, Days and Seasons (ASCENDS). 2 micron laser is a viable IPDA transmitter to measure CO2 and H2O column density from space. The objective is to demonstrate a first airborne direct detection 2 micron IPDA lidar for CO2 and H2O measurements.

Neuronal Dynamics and Axonal Flow, V. The Semisolid State of the Moving Axonal Column

PubMed Central

Weiss, Paul A.

1972-01-01

Evidence assembled since the first comprehensive description of “axonal flow”, by deformation analysis, electron microscopy, cinemicrography, and microrheology, has confirmed that the axon of the mature neuron is (a) a semisolid column; (b) in cellulifugal motion at about 1 μm/min (1 mm per day); (c) continuously reproduced at its perikaryal base; (d) propelled by a microperistaltic pulse wave in its surface; and (e) undergoing internal dissolution at the nerve ending. The axon thus “flows” as a structural entity (“axonal flow”), in contradistinction to fast “intraaxonal transport” of molecules and molecular assemblies along internal routes and by mechanisms that are still unknown. Images PMID:4111049

Tunable Single-Frequency Near IR Lasers for DIAL Applications

NASA Technical Reports Server (NTRS)

Henderson, Sammy W.; Marquardt, John H.; Carrig, Timothy J.; Gatt, Phil; Smith, Duane D.; Hale, Charley P.

2000-01-01

Tunable single-frequency sources in the 2-4 micron wavelength region are useful for remote DIAL measurements of chemicals and pollutants. We are developing tunable single-frequency transmitters and receivers for both direct and coherent detection lidar measurement applications. We have demonstrated a direct-diode-pumped PPLN-based OPO that operates single frequency, produces greater than 10 mW cw and is tunable over the 2.5 - 3.9 micron wavelength region. This laser has been used to injection seed a pulsed PPLN OPO, pumped by a 1.064 micron Nd:YAG laser, producing 50-100 microJoule single-frequency pulses at 100 Hz PRF near 3.6 micron wavelength. In addition, we have demonstrated a cw Cr:ZnSe laser that is tunable over the 2.1 - 2.8 micron wavelength region. This laser is pumped by a cw diode-pumped Tm:YALO laser and has produced over 1.8 W cw. Tm- and Tm, Ho-doped single-frequency solid-state lasers that produce over 50 mW cw and are tunable over approximately 10 nm in the 2 -2.1 micron band with fast PZT tuning have also been demonstrated. A fast PZT-tunable Tm, Ho:YLF laser was used for a direct-detection column content DIAL measurement of atmospheric CO2. Modeling shows that that all these cw and pulsed sources are useful for column-content coherent DIAL measurements at several km range using topographic targets.

Pulse Profiles, Accretion Column Dips and a Flare in GX 1+4 During a Faint State

NASA Technical Reports Server (NTRS)

Giles, A. B.; Galloway, D. K.; Greenhill, J. G.; Storey, M. C.; Wilson, C. A.

1999-01-01

The Rossi X-ray Timing Explorer (RXTE) spacecraft observed the X-ray GX 1+4 for it period of 34 hours on July 19/20 1996. The source faded front an intensity of approximately 20 mcrab to a minimum of <= 0.7 mcrab and then partially recovered towards the end of the observation. This extended minimum lasted approximately 40,000 seconds. Phase folded light curves at a barycentric rotation period of 124.36568 +/- 0.00020 seconds show that near the center of the extended minimum the source stopped pulsing in the traditional sense but retained a weak dip feature at the rotation period. Away from the extended minimum the dips are progressively narrower at higher energies and may be interpreted as obscurations or eclipses of the hot spot by the accretion column. The pulse profile changed from leading-edge bright before the extended minimum to trailing-edge bright after it. Data from the Burst and Transient Source Experiment (BATSE) show that a torque reversal occurred < 10 days after our observation. Our data indicate that the observed rotation departs from a constant period with a P/P value of approximately -1.5% per year at a 4.5sigma significance. We infer that we may have serendipitously obtained data, with high sensitivity and temporal resolution about the time of an accretion disk spin reversal. We also observed a rapid flare which had some precursor activity close to the center of the extended minimum.

[Simultaneous determination of pesticide residues in agricultural products by LC-MS/MS].

PubMed

Watanabe, Minae; Ueno, Eiji; Inoue, Tomomi; Ohno, Haruka; Ikai, Yoshitomo; Morishita, Toshio; Oshima, Harumi; Hayashi, Rumiko

2013-01-01

A method for the simultaneous determination of multiple pesticide residues in agricultural products was developed by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). The sample was extracted with acetonitrile. Co-extractives were removed by GPC/graphitized carbon column SPE, and silica gel/PSA cartridge column SPE. Pesticides in the test solution were determined by LC-MS/MS using scheduled MRM. Recoveries of 124 pesticides from spinach, brown rice, soybean, orange and tomato were tested at the level of 0.1 µg/g, and those of 121 pesticides ranged from 70 to 120% (RSD≤15%). Pesticide residues in 239 agricultural products were investigated by this method, and residues of 49 pesticides were detected in 98 agricultural products.

Clustering header categories extracted from web tables

NASA Astrophysics Data System (ADS)

Nagy, George; Embley, David W.; Krishnamoorthy, Mukkai; Seth, Sharad

2015-01-01

Revealing related content among heterogeneous web tables is part of our long term objective of formulating queries over multiple sources of information. Two hundred HTML tables from institutional web sites are segmented and each table cell is classified according to the fundamental indexing property of row and column headers. The categories that correspond to the multi-dimensional data cube view of a table are extracted by factoring the (often multi-row/column) headers. To reveal commonalities between tables from diverse sources, the Jaccard distances between pairs of category headers (and also table titles) are computed. We show how about one third of our heterogeneous collection can be clustered into a dozen groups that exhibit table-title and header similarities that can be exploited for queries.

Curcuma longa extract as a histological dye for collagen fibres and red blood cells

PubMed Central

Avwioro, O G; Onwuka, S K; Moody, J O; Agbedahunsi, J M; Oduola, T; Ekpo, O E; Oladele, A A

2007-01-01

Crude ethanolic extract and column chromatographic fractions of the Allepey cultivar of Curcuma longa Roxb, commonly called turmeric (tumeric) in commerce, were used as a stain for tissue sections. Staining was carried out under basic, acidic and neutral media conditions. Inorganic and organic dissolution solvents were used. The stain was used as a counterstain after alum and iron haematoxylins. C. longa stained collagen fibres, cytoplasm, red blood cells and muscle cells yellow. It also stained in a fashion similar to eosin, except for its intense yellow colour. Preliminary phytochemical evaluation of the active column fraction revealed that it contained flavonoids, free anthraquinone and deoxy sugar. A cheap, natural dye can thus be obtained from C. longa. PMID:17451535

100 s extraction of negative ion beams by using actively temperature-controlled plasma grid

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

Kojima, A., E-mail: kojima.atsushi@jaea.go.jp; Hanada, M.; Yoshida, M.

2014-02-15

Long pulse beam extraction with a current density of 120 A/m{sup 2} for 100 s has been achieved with a newly developed plasma grid (PG) for the JT-60SA negative ion source which is designed to produce high power and long pulse beams with a negative ion current of 130 A/m{sup 2} (22 A) and a pulse length of 100 s. The PG temperature is regulated by fluorinated fluids in order to keep the high PG temperature for the cesium-seeded negative ion production. The time constant for temperature controllability of the PG was measured to be below 10 s, which wasmore » mainly determined by the heat transfer coefficient of the fluorinated fluid. The measured decay time of the negative ion current extracted from the actively temperature-controlled PG was 430 s which was sufficient for the JT-60SA requirement, and much longer than that by inertial-cooling PG of 60 s. Obtained results of the long pulse capability are utilized to design the full size PG for the JT-60SA negative ion source.« less

Optimization of pulsed ultrasound-assisted technique for extraction of phenolics from pomegranate peel of Malas variety: Punicalagin and hydroxybenzoic acids.

PubMed

Kazemi, Milad; Karim, Roselina; Mirhosseini, Hamed; Abdul Hamid, Azizah

2016-09-01

Pomegranate peel is a rich source of phenolic compounds (such as punicalagin and hydroxybenzoic acids). However, the content of such bioactive compounds in the peel extract can be affected by extraction type and condition. It was hypothesized that the optimization of a pulsed ultrasound-assisted extraction (PUAE) technique could result in the pomegranate peel extract with higher yield and antioxidant activity. The main goal was to optimize PUAE condition resulting in the highest yield and antioxidant activity as well as the highest contents of punicalagin and hydroxybenzoic acids. The operation at the intensity level of 105W/cm(2) and duty cycle of 50% for a short time (10min) had a high efficiency for extraction of phenolics from pomegranate peel. The application of such short extraction can save the energy and cost of the production. Punicalagin and ellagic acid were the most predominant phenolic compounds quantified in the pomegranate peel extract (PPE) from Malas variety. PPE contained a minor content of gallic acid. Copyright © 2016 Elsevier Ltd. All rights reserved.

Mechanistic study of lead desorption during the leaching process of ion-absorbed rare earths: pH effect and the column experiment

NASA Astrophysics Data System (ADS)

Xue, Q.; Tang, J., Sr.; Chen, H.

2017-12-01

High concentrations of ammonium sulfate, often used in the in-situ mining process, can result in a decrease of pH in the environment and dissolution of rare earth metals. Ammonium sulfate can also cause desorption of toxic heavy metals, leading to environmental and human health implications. In this study, the desorption behavior and fraction changes of lead in the ion-absorbed rare earth ore were studied using batch desorption experiments and column leaching tests. Results from batch desorption experiments showed that the desorption process of lead included fast and slow stages, and followed an Elovich model well. The desorption rate and the proportion of lead content in the solution to the total lead in the soil were observed to increase with a decrease in the initial pH of the ammonium sulfate solution. The lead in soil included an acid extractable fraction, reducible fraction, oxidizable fraction, and a residual fraction, with the predominant fractions being the reducible and acid extractable fractions. 96% of the extractable fraction in soil were desorbed into solution at pH=3.0, and the content of the reducible fraction was observed to initially increase (when pH>4.0) and then decrease (when pH<4.0) with a decrease in pH. Column leaching tests indicated that the content of lead in the different fractions of soil followed the trend of reducible fraction > oxidizable fraction > acid extractable fraction > residual fraction after the simulating leaching mining process. The change in pH was also found to have a larger influence on the acid extractable and reducible fractions than the other two fractions. The proportion of the extractable fraction being leached was ca. 86%, and the reducible fraction was enriched along the migration direction of the leaching liquid. These results suggest that certain lead fractions may desorb again and contaminate the environment via acid rain, which provides significant information for environmental assessment and remediation after mining process.

Testing of nylon 6 nanofibers with different surface densities as sorbents for solid phase extraction and their selectivity comparison with commercial sorbent.

PubMed

Háková, Martina; Raabová, Hedvika; Havlíková, Lucie Chocholoušová; Chocholouš, Petr; Chvojka, Jiří; Šatínský, Dalibor

2018-05-01

Nylon 6 nanofibers were tested for their ability to serve as a sorbent for solid phase extraction (SPE). The regular nanostructure providing a great sorption area and amidic functionality should lead to the assumption that nylon 6 nanofibers could be used as a novel sorbent with great potential for sample pre-treatment. However, due to the substantial differences between classical particle sorbents used for solid phase extraction and nanofibers, it is necessary to evaluate this novel approach. This article describes three types of laboratory fabricated nylon 6 nanofibers with different surface density (5.04gm -2 , 3.90gm -2 and 0.75gm -2 ) and corresponding surface areas for solid phase extraction of several groups of compounds with different structural and physicochemical properties (parabens, steroids, flavonoids and pesticides). The nanofibers were created by needleless electrospinning. Extraction columns were manually packed in classic 1- or 3-mL plastic syringe cartridges with 26-30mg of nanofibers and the column bed was sealed with polypropylene frits. The SPE procedure followed a typical five-step protocol and the collected eluates were analyzed by HPLC with UV detection. Extraction recovery was used as a parameter to evaluate the behavior of the analytes within the SPE process. Under this set condition, the recovery of the SPE process ranged from 23.1% to 125.8%. SPE showed good repeatability (0.58-11.87% RSD) and inter-day reproducibility (3.86-9.79% RSD). The achieved results were compared with SPE using a classic particle sorbent column. Good mechanical and chemical stability of nanofibers was proved. Scanning electron microscope was used for the evaluation of morphological changes in nanostructure. Nylon 6 nanofibers proved being a cost-effective sorbent for repeated use in SPE. Nylon 6 nanofibers have great potential in miniaturized SPE enabling users to overcome troubles with high back-pressure. Copyright © 2018 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.

Instrument for Solvent Extraction and Analysis (ISEE) of Organics from Regolith Simulant Using Supercritical Fluid Extraction and Chromatography

NASA Technical Reports Server (NTRS)

Franco, Carolina; Hintze, Paul E.

2017-01-01

ISEE is an instrument with the potential to perform extractions from regolith found on the surface of asteroids and planets, followed by characterization and quantitation of the extracts using supercritical fluid extraction (SFE) and chromatography (SFC). SFE is a developed technique proven to extract a wide range of organic compounds. SFC is similar to High Performance Liquid Chromatography (HPLC) but has the advantage of performing chiral separations without needing to derivatize the chiral compounds. CO2 will be the solvent for both stages as it is readily available in the Mars atmosphere. ISEE will capture CO2 from the environment, and use it for SFE and SFC. If successful, this would allow ISEE to perform analysis of organic compounds without using consumables. This paper will present results on a preliminary, proof-of-principle effort to use SFE and SFC to extract and analyze lunar regolith simulant spiked with organic compounds representing a range of organics that ISEE would expect to characterize. An optimization of variables for the extraction of the organics from the spiked regolith was successfully developed, using 138 bar pressure and 40 C temperature. The extraction flow rate was optimized at 2% SLPM with 30% methanol modifier. The extractions were successful with a value of 77.3+/- 0.9% of organics extracted. However, the recovery of organics after the extraction was very low with only 48.5+/-14.2%. Moreover, three columns were selected to analyze multiple samples at a time; two of them are Viridis HSS C18 SB and Torus DIOL, and the third column, specific for chiral separations, has not yet been selected yet.

The effect of dilution and the use of a post-extraction nucleic acid purification column on the accuracy, precision, and inhibition of environmental DNA samples

USGS Publications Warehouse

Mckee, Anna M.; Spear, Stephen F.; Pierson, Todd W.

2015-01-01

Isolation of environmental DNA (eDNA) is an increasingly common method for detecting presence and assessing relative abundance of rare or elusive species in aquatic systems via the isolation of DNA from environmental samples and the amplification of species-specific sequences using quantitative PCR (qPCR). Co-extracted substances that inhibit qPCR can lead to inaccurate results and subsequent misinterpretation about a species’ status in the tested system. We tested three treatments (5-fold and 10-fold dilutions, and spin-column purification) for reducing qPCR inhibition from 21 partially and fully inhibited eDNA samples collected from coastal plain wetlands and mountain headwater streams in the southeastern USA. All treatments reduced the concentration of DNA in the samples. However, column purified samples retained the greatest sensitivity. For stream samples, all three treatments effectively reduced qPCR inhibition. However, for wetland samples, the 5-fold dilution was less effective than other treatments. Quantitative PCR results for column purified samples were more precise than the 5-fold and 10-fold dilutions by 2.2× and 3.7×, respectively. Column purified samples consistently underestimated qPCR-based DNA concentrations by approximately 25%, whereas the directional bias in qPCR-based DNA concentration estimates differed between stream and wetland samples for both dilution treatments. While the directional bias of qPCR-based DNA concentration estimates differed among treatments and locations, the magnitude of inaccuracy did not. Our results suggest that 10-fold dilution and column purification effectively reduce qPCR inhibition in mountain headwater stream and coastal plain wetland eDNA samples, and if applied to all samples in a study, column purification may provide the most accurate relative qPCR-based DNA concentrations estimates while retaining the greatest assay sensitivity.

The feature extraction of "cat-eye" targets based on bi-spectrum

NASA Astrophysics Data System (ADS)

Zhang, Tinghua; Fan, Guihua; Sun, Huayan

2016-10-01

In order to resolve the difficult problem of detection and identification of optical targets in complex background or in long-distance transmission, this paper mainly study the range profiles of "cat-eye" targets using bi-spectrum. For the problems of laser echo signal attenuation serious and low Signal-Noise Ratio (SNR), the multi-pulse laser signal echo signal detection algorithm which is based on high-order cumulant, filter processing and the accumulation of multi-pulse is proposed. This could improve the detection range effectively. In order to extract the stable characteristics of the one-dimensional range profile coming from the cat-eye targets, a method is proposed which extracts the bi-spectrum feature, and uses the singular value decomposition to simplify the calculation. Then, by extracting data samples of different distance, type and incidence angle, verify the stability of the eigenvector and effectiveness extracted by bi-spectrum.

Solid-state pulse modulator using Marx generator for a medical linac electron-gun

NASA Astrophysics Data System (ADS)

Lim, Heuijin; Hyeok Jeong, Dong; Lee, Manwoo; Lee, Mujin; Yi, Jungyu; Yang, Kwangmo; Ro, Sung Chae

2016-04-01

A medical linac is used for the cancer treatment and consists of an accelerating column, waveguide components, a magnetron, an electron-gun, a pulse modulator, and an irradiation system. The pulse modulator based on hydrogen thyratron-switched pulse-forming network is commonly used in linac. As the improvement of the high power semiconductors in switching speed, voltage rating, and current rating, an insulated gate bipolar transistor has become the more popular device used for pulsed power systems. We propose a solid-state pulse modulator to generator high voltage by multi-stacked storage-switch stages based on the Marx generator. The advantage of our modulator comes from the use of two semiconductors to control charging and discharging of the storage capacitor at each stage and it allows to generate the pulse with various amplitudes, widths, and shapes. In addition, a gate driver for two semiconductors is designed to reduce the control channels and to protect the circuits. It is developed for providing the pulsed power to a medical linac electron-gun that requires 25 kV and 1 A as the first application. In order to improve the power efficiency and achieve the compactness modulator, a capacitor charging power supply, a Marx pulse generator, and an electron-gun heater isolated transformer are constructed and integrated. This technology is also being developed to extend the high power pulsed system with > 1 MW and also other applications such as a plasma immersed ion implantation and a micro pulse electrostatic precipitator which especially require variable pulse shape and high repetition rate > 1 kHz. The paper describes the design features and the construction of this solid-state pulse modulator. Also shown are the performance results into the linac electron-gun.

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.

Suitability of DPPH spiking for antioxidant screening in natural products: the example of galloyl derivatives from red maple bark extract.

PubMed

Geoffroy, Thibaud R; Meda, Naamwin R; Stevanovic, Tatjana

2017-09-01

To investigate the antioxidant potential in natural products, radical scavenging tests (ABTS, DPPH, ORAC, etc.) are usually considered as the first approach. In addition to the standard colorimetric assays, methods using separation techniques (on-line and pre-column assays) have been developed in the past decades. Based on the peak area (PA) reductions of compounds monitored by HPLC, the pre-column spiking method allows rapid characterisation of natural matrices avoiding laborious isolation steps. However, available information about the significance of the results produced remains scarce. Here, we report, for the first time, a discussion of the potential of the pre-column DPPH spiking method to pinpoint antioxidant compounds using red maple bark extract (RMBE). First, DPPH spiking was conventionally applied to the galloyl compounds in the extract showing the inadequacy of assessing results by PA reductions. The method was then applied to pure galloyl derivatives, evaluating their molar amount reacted (MAR) for more significance. The comparison with the standard DPPH-HPLC/AE method directly monitoring DPPH • inhibition highlighted the inability to retrieve the respective antioxidant efficiencies (AE) of each compound by using DPPH spiking. Despite its limitations, the DPPH spiking method brought to light an autoxidation phenomenon and a matrix/mixture effect investigated through tertiary mixtures of galloyl compounds. Although restricted to the compounds from one natural matrix, this study questions the validity of the spiking method as usually performed and could serve as a basis for further investigations (explorations of other natural products, kinetics considerations). Graphical abstract Investigation of the pre-column DPPH spiking method through the case of galloyl derivatives.

Development of a Multiple-Stage Differential Mobility Analyzer (MDMA)

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

Chen, Da-Ren; Cheng, Mengdawn

2007-01-01

A new DMA column has been designed with the capability of simultaneously extracting monodisperse particles of different sizes in multiple stages. We call this design a multistage DMA, or MDMA. A prototype MDMA has been constructed and experimentally evaluated in this study. The new column enables the fast measurement of particles in a wide size range, while preserving the powerful particle classification function of a DMA. The prototype MDMA has three sampling stages, capable of classifying monodisperse particles of three different sizes simultaneously. The scanning voltage operation of a DMA can be applied to this new column. Each stage ofmore » MDMA column covers a fraction of the entire particle size range to be measured. The covered size fractions of two adjacent stages of the MDMA are designed somewhat overlapped. The arrangement leads to the reduction of scanning voltage range and thus the cycling time of the measurement. The modular sampling stage design of the MDMA allows the flexible configuration of desired particle classification lengths and variable number of stages in the MDMA. The design of our MDMA also permits operation at high sheath flow, enabling high-resolution particle size measurement and/or reduction of the lower sizing limit. Using the tandem DMA technique, the performance of the MDMA, i.e., sizing accuracy, resolution, and transmission efficiency, was evaluated at different ratios of aerosol and sheath flowrates. Two aerosol sampling schemes were investigated. One was to extract aerosol flows at an evenly partitioned flowrate at each stage, and the other was to extract aerosol at a rate the same as the polydisperse aerosol flowrate at each stage. We detail the prototype design of the MDMA and the evaluation result on the transfer functions of the MDMA at different particle sizes and operational conditions.« less

QTLTableMiner++: semantic mining of QTL tables in scientific articles.

PubMed

Singh, Gurnoor; Kuzniar, Arnold; van Mulligen, Erik M; Gavai, Anand; Bachem, Christian W; Visser, Richard G F; Finkers, Richard

2018-05-25

A quantitative trait locus (QTL) is a genomic region that correlates with a phenotype. Most of the experimental information about QTL mapping studies is described in tables of scientific publications. Traditional text mining techniques aim to extract information from unstructured text rather than from tables. We present QTLTableMiner ++ (QTM), a table mining tool that extracts and semantically annotates QTL information buried in (heterogeneous) tables of plant science literature. QTM is a command line tool written in the Java programming language. This tool takes scientific articles from the Europe PMC repository as input, extracts QTL tables using keyword matching and ontology-based concept identification. The tables are further normalized using rules derived from table properties such as captions, column headers and table footers. Furthermore, table columns are classified into three categories namely column descriptors, properties and values based on column headers and data types of cell entries. Abbreviations found in the tables are expanded using the Schwartz and Hearst algorithm. Finally, the content of QTL tables is semantically enriched with domain-specific ontologies (e.g. Crop Ontology, Plant Ontology and Trait Ontology) using the Apache Solr search platform and the results are stored in a relational database and a text file. The performance of the QTM tool was assessed by precision and recall based on the information retrieved from two manually annotated corpora of open access articles, i.e. QTL mapping studies in tomato (Solanum lycopersicum) and in potato (S. tuberosum). In summary, QTM detected QTL statements in tomato with 74.53% precision and 92.56% recall and in potato with 82.82% precision and 98.94% recall. QTM is a unique tool that aids in providing QTL information in machine-readable and semantically interoperable formats.

Analytical methods for the determination of urinary 2,4-dichlorophenoxyacetic acid and 2-methyl-4-chlorophenoxyacetic acid in occupationally exposed subjects and in the general population.

PubMed

Aprea, C; Sciarra, G; Bozzi, N

1997-01-01

Two methods for the quantitative analysis of 2,4-dichlorophenoxyacetic acid (2,4-D) and 2-methyl-4-chlorophenoxyacetic acid (MCPA) in urine were compared. The first was an high-performance liquid chromatography method using a C8 column with ion suppression and diode array detection. The urine extracts were first purified by solid-phase extraction (SPE) on silica capillary columns. The detection limit of the method was 15 micrograms/L for both compounds. The percentage coefficient of variation of the whole analysis evaluated at a concentration of 125.0 micrograms/L was 6.2% for 2,4-D and 6.8% for MCPA. The mean recovery of analysis was 81% for 2,4-D and 85% for MCPA. The second was a gas chromatographic (GC) method in which the compounds were first derivatized with pentafluorobenzylbromide to pentafluorobenzyl esters, which were determined with a slightly polar capillary column and electron capture detection. Before GC analysis, the urine extracts were purified by SPE on silica capillary columns. This method had a detection limit of 1 microgram/L for both compounds and a percentage coefficient of variation of the whole analysis, evaluated at a concentration of 30.0 micrograms/L, of 8% for 2,4-D, and of 5.5% for MCPA. the mean recovery was 87% for 2,4-D and 94% for MCPA. The low detection limit made the second method suitable for assaying the two herbicides in the general population. Duplicate analysis of ten urine samples from occupationally exposed subjects by the two methods gave identical results for a wide range of concentrations.

Agricultural and Food Processing Applications of Pulsed Power and Plasma Technologies

NASA Astrophysics Data System (ADS)

Takaki, Koichi

Agricultural and food processing applications of pulsed power and plasma technologies are described in this paper. Repetitively operated compact pulsed power generators with a moderate peak power are developed for the agricultural and the food processing applications. These applications are mainly based on biological effects and can be categorized as germination control of plants such as Basidiomycota and arabidopsis inactivation of bacteria in soil and liquid medium of hydroponics; extraction of juice from fruits and vegetables; decontamination of air and liquid, etc. Types of pulsed power that have biological effects are caused with gas discharges, water discharges, and electromagnetic fields. The discharges yield free radicals, UV radiation, intense electric field, and shock waves. Biologically based applications of pulsed power and plasma are performed by selecting the type that gives the target objects the adequate result from among these agents or byproducts. For instance, intense electric fields form pores on the cell membrane, which is called electroporation, or influence the nuclei. This paper mainly describes the application of the pulsed power for the germination control of Basidiomycota i.e. mushroom, inactivation of fungi in the soil and the liquid medium in hydroponics, and extraction of polyphenol from skins of grape.

Understanding the mechanisms of lipid extraction from microalga Chlamydomonas reinhardtii after electrical field solicitations and mechanical stress within a microfluidic device.

PubMed

Bensalem, Sakina; Lopes, Filipa; Bodénès, Pierre; Pareau, Dominique; Français, Olivier; Le Pioufle, Bruno

2018-06-01

One way envisioned to overcome part of the issues biodiesel production encounters today is to develop a simple, economically viable and eco-friendly process for the extraction of lipids from microalgae. This study investigates the lipid extraction efficiency from the microalga Chlamydomonas reinhardtii as well as the underlying mechanisms. We propose a new methodology combining a pulsed electric field (PEF) application and mechanical stresses as a pretreatment to improve lipid extraction with solvents. Cells enriched in lipids are therefore submitted to electric field pulses creating pores on the cell membrane and then subjected to a mechanical stress by applying cyclic pressures on the cell wall (using a microfluidic device). Results showed an increase in lipid extraction when cells were pretreated by the combination of both methods. Microscopic observations showed that both pretreatments affect the cell structure. Finally, the dependency of solvent lipid extraction efficiency with the cell wall structure is discussed. Copyright © 2018 Elsevier Ltd. All rights reserved.

Liquid chromatography coupled to different atmospheric pressure ionization sources-quadrupole-time-of-flight mass spectrometry and post-column addition of metal salt solutions as a powerful tool for the metabolic profiling of Fusarium oxysporum.

PubMed

Cirigliano, Adriana M; Rodriguez, M Alejandra; Gagliano, M Laura; Bertinetti, Brenda V; Godeas, Alicia M; Cabrera, Gabriela M

2016-03-25

Fusarium oxysporum L11 is a non-pathogenic soil-borne fungal strain that yielded an extract that showed antifungal activity against phytopathogens. In this study, reversed-phase high-performance liquid chromatography (RP-HPLC) coupled to different atmospheric pressure ionization sources-quadrupole-time-of-flight mass spectrometry (API-QTOF-MS) was applied for the comprehensive profiling of the metabolites from the extract. The employed sources were electrospray (ESI), atmospheric pressure chemical ionization (APCI) and atmospheric pressure photoionization (APPI). Post-column addition of metal solutions of Ca, Cu and Zn(II) was also tested using ESI. A total of 137 compounds were identified or tentatively identified by matching their accurate mass signals, suggested molecular formulae and MS/MS analysis with previously reported data. Some compounds were isolated and identified by NMR. The extract was rich in cyclic peptides like cyclosporins, diketopiperazines and sansalvamides, most of which were new, and are reported here for the first time. The use of post-column addition of metals resulted in a useful strategy for the discrimination of compound classes since specific adducts were observed for the different compound families. This technique also allowed the screening for compounds with metal binding properties. Thus, the applied methodology is a useful choice for the metabolic profiling of extracts and also for the selection of metabolites with potential biological activities related to interactions with metal ions. Copyright © 2015 Elsevier B.V. All rights reserved.

Micellar liquid chromatographic determination of arbutin and hydroquinone in medicinal plant extracts and commercial cosmetic products.

PubMed

Thogchai, W; Liawruangrath, B

2013-06-01

A simple micellar liquid chromatographic (MLC) procedure for simultaneous determination of arbutin and hydroquinone in medicinal plant extracts and commercial cosmetic products was proposed. This method was developed and validated. The chromatographic conditions were also optimized. All analyses were performed at room temperature in an isocratic mode, using a mixture of 1% (v/v) acetonitrile and 0.006 mol L⁻¹ Brij 35 (pH 6.0) as a mobile phase. The flow rate was set at 1.0 mL min⁻¹. The analytical column was a 150 × 3.9 mm Nova-Pak C-18 column. The effluent from the analytical column was monitored by UV detection at 280 nm. Under the optimum conditions, arbutin and hydroquinone could be determined within a concentration range of 2-50 μg mL⁻¹ of arbutin, and hydroquinone was obtained with the regression equations; y = 0.045x + 0.042 (r² = 0.9923) and y = 0.091x + 0.050 (r² = 0.9930) respectively. The limits of detection were found to be 0.51 μg mL⁻¹ and 0.37 μg mL⁻¹ for arbutin and hydroquinone respectively. The proposed MLC method was applied for the determination of arbutin and hydroquinone contents in medicinal plant extracts and commercial cosmetic products. This proposed MLC method is thus suitable for routine analysis of arbutin and hydroquinone in the pharmaceutical formulations, cosmetic products and raw medicinal plant extracts. ICS © 2013 Society of Cosmetic Scientists and the Société Française de Cosmétologie.

Quantitation of anticonvulsant drugs in serum by gas-chromatography on the stationary phase SP-2510.

PubMed

Godolphin, W; Thoma, J

1978-03-01

A new column packing, SP-2510 DA (Supelco, Inc., Bellefonte, Pa. 16823), is an excellent stationary phase for the determination of a wide variety of anticonvulsant drugs by gas--liquid chromatography without derivatization. However, when uncomplicated extraction procedures are used, serum cholesterol interferes with the determination of primidone. By the simple expedient of adding a short "pre-column" containing another phase (SP-2250 DA) the problem is overcome.

Quantitative high-performance liquid chromatographic determination of retinoids in human serum using on-line solid-phase extraction and column switching. Determination of 9-cis-retinoic acid, 13-cis-retinoic acid, all-trans-retinoic acid, 4-oxo-all-trans-retinoicacid and 4-oxo-13-cis-retinoic acid.

PubMed

Gundersen, T E; Lundanes, E; Blomhoff, R

1997-03-28

A fully automated isocratic high-performance liquid chromatographic method for the determination of 9-cis-retinoic acid, 13-cis-retinoic acid, all-trans-retinoic acid, 4-oxo-13-cis-retinoic acid and 4-oxo-all-trans-retinoic acid, has been developed using on-line solid-phase extraction and a column switching technique allowing clean-up and pre-concentration in a single step. A 500-microliter sample of serum was diluted with 750 microliters of a solution containing 20% acetonitrile and the internal standard 9,10-dimethylanthracene. About 1000 microliters of this mixture was injected on a 20 x 4.6 mm I.D. poly ether ether ketone (PEEK) pre-column with titanium frits packed with Bondapak C18, 37-53 microns, 300 A particles. Proteins and very polar compounds were washed out to waste, from the pre-column, with 0.05% trifluoroacetic acid (TFA)-acetonitrile (8.5:1.5, v/v). More than 200 aliquots of diluted serum could be injected on this pre-column before elevated back-pressure enforces replacement. Components retained on the pre-column were backflushed to the analytical column for separation and detection at 360 nm. Baseline separation was achieved using a single 250 x 4.6 mm I.D. Suplex pKb-100 column and a mobile phase containing 69:10:2:16:3 (v/v) of acetonitrile-methanol-n-butanol-2% ammonium acetate-glacial acetic acid. A total time of analysis of less than 30 min, including sample preparation, was achieved. Recoveries were in the range of 79-86%. The limit of detection was 1-7 ng/ml serum and the precision, in the concentration range 20-1000 ng/ml, was between 1.3 and 4.5% for all five compounds. The method was applied for the analysis of human serum after oral administration of 60 mg Roaccutan. The method is well suited for pharmacological studies, while the endogenous levels of some retinoic acid isomers are below the limit of quantitation.

Fifteen terawatt picosecond CO2 laser system.

PubMed

Haberberger, D; Tochitsky, S; Joshi, C

2010-08-16

The generation of a record peak-power of 15 TW (45 J, 3 ps) in a single CO(2) laser beam is reported. Using a master oscillator-power amplifier laser system, it is shown that up to 100 J of energy can be extracted in a train of 3 ps laser pulses separated by 18 ps, a characteristic time of the CO(2) molecule. The bandwidth required for amplifying the short injected laser pulse train in a 2.5 atm final CO(2) amplifier is provided by field broadening of the medium at intensities of up to 140 GW/cm(2). The measured saturation energy for 3 ps pulses is 120 mJ/cm(2) which confirms that energy is simultaneously extracted from six rovibrational lines.

Looking at A 0535+26 at low luminosities with NuSTAR

NASA Astrophysics Data System (ADS)

Ballhausen, Ralf; Pottschmidt, Katja; Fürst, Felix; Wilms, Jörn; Tomsick, John A.; Schwarm, Fritz-Walter; Stern, Daniel; Kretschmar, Peter; Caballero, Isabel; Harrison, Fiona A.; Boggs, Steven E.; Christensen, Finn E.; Craig, William W.; Hailey, Charles J.; Zhang, William W.

2017-12-01

We report on two NuSTAR observations of the high-mass X-ray binary A 0535+26 taken toward the end of its normal 2015 outburst at very low 3-50 keV luminosities of 1.4 × 1036 erg s-1 and 5 × 1035 erg s-1, which are complemented by nine Swift observations. The data clearly confirm indications seen in earlier data that the source's spectral shape softens as it becomes fainter. The smooth exponential rollover at high energies seen in the first observation evolves to a much more abrupt steepening of the spectrum at 20-30 keV. The continuum evolution can be nicely described with emission from a magnetized accretion column, modeled using the compmag model modified by an additional Gaussian emission component for the fainter observation. Between the two observations, the optical depth changes from 0.75 ± 0.04 to , the electron temperature remains constant, and there is an indication that the column decreases in radius. Since the energy-resolved pulse profiles remain virtually unchanged in shape between the two observations, the emission properties of the accretion column reflect the same accretion regime. This conclusion is also confirmed by our result that the energy of the cyclotron resonant scattering feature (CRSF) at 45 keV is independent of the luminosity, implying that the magnetic field in the region in which the observed radiation is produced is the same in both observations. Finally, we also constrain the evolution of the continuum parameters with the rotational phase of the neutron star. The width of the CRSF could only be constrained for the brighter observation. Based on Monte Carlo simulations of CRSF formation in single accretion columns, its pulse phase dependence supports a simplified fan beam emission pattern. The evolution of the CRSF width is very similar to that of the CRSF depth, which is, however, in disagreement with expectations.

Development of "ultrasound-assisted dynamic extraction" and its combination with CCC and CPC for simultaneous extraction and isolation of phytochemicals.

PubMed

Zhang, Yuchi; Liu, Chunming; Li, Jing; Qi, Yanjuan; Li, Yuchun; Li, Sainan

2015-09-01

A new method for the extraction of medicinal herbs termed ultrasonic-assisted dynamic extraction (UADE) was designed and evaluated. This technique was coupled with counter-current chromatography (CCC) and centrifugal partition chromatography (CPC) and then applied to the continuous extraction and online isolation of chemical constituents from Paeonia lactiflora Pall (white peony) roots. The mechanical parameters, including the pitch and diameter of the shaft, were optimized by means of mathematical modeling. Furthermore, the configuration and mechanism of online UADE coupled with CCC and CPC were elaborated. The stationary phases of the two-phase solvent systems from CCC and CPC were utilized as the UADE solution. The extraction solution was pumped into the sample loop and then introduced into the CCC column; the target compounds were eluted with the lower aqueous phase of the two-phase solvent system. During the CCC separation, the extraction solution was continuously fed in the sample loop by turning the ten-port valve; the extraction solution was then pumped into the CPC column and eluted by the mobile phase of the two-phase solvent system mentioned above. When the first cycle of the UADE/CCC/CPC was completed, the second cycle experiment could be carried out, and so on. Four target compounds (albiflorin, benzoylpaeoniflorin, paeoniflorin, and galloylpaeoniflorin) with purities above 94.96% were successfully extracted and isolated online using the two-phase solvent system comprising ethyl acetate-n-butanol-ethanol-water (1:3.5:2:4.5, v/v/v/v). Compared with conventional extraction methods, the instrumental setup of the present method offers the advantages of automation and systematic extraction and isolation of natural products. Crown Copyright © 2015. Published by Elsevier B.V. All rights reserved.

Separation, purification, and α-glucosidase inhibition of polysaccharides from Coriolus versicolor LH1 mycelia.

PubMed

Hsu, Wen-kuang; Hsu, Tai-hao; Lin, Fang-yi; Cheng, Yuan-kai; Yang, John Po-wen

2013-01-30

Intracellular polysaccharides (iPs) were separated and purified from Coriolus versicolor LH1 mycelia and characterized for their α-glucosidase inhibitory properties. Three iP fractions (iPL-F5-2-1, iPL-F5-4-1, and iPL-F5-5-1) were extracted, separated, and purified from LH1 mycelia using microwave extraction technology, a DEAE-Sepharose CL-6B column, a Diaion HP20 macroporous adsorption column, and a Sephadex™ G-50 gel-permeation column. The principal constituents of iPL-F5-2-1, iPL-F5-4-1, and iPL-F5-5-1 were saponins and polyphenoic compound mixtures. The enzyme inhibition activity, IC(50) values, of these three fractions were 1.7, 1.8, and 0.8 mg/mL, respectively. The α-glucosidase inhibitory properties were related to the presence of α-(1,4) glycosidic linkages in the polysaccharide structure and the total relative percentage of d-glucose and d-galactose in the structure of polysaccharides, other than triterpenoids. Copyright © 2012 Elsevier Ltd. All rights reserved.

Pilot-scale resin adsorption as a means to recover and fractionate apple polyphenols.

PubMed

Kammerer, Dietmar R; Carle, Reinhold; Stanley, Roger A; Saleh, Zaid S

2010-06-09

The purification and fractionation of phenolic compounds from crude plant extracts using a food-grade acrylic adsorbent were studied at pilot-plant scale. A diluted apple juice concentrate served as a model phenolic solution for column adsorption and desorption trials. Phenolic concentrations were evaluated photometrically using the Folin-Ciocalteu assay and by HPLC-DAD. Recovery rates were significantly affected by increasing phenolic concentrations of the feed solutions applied to the column. In contrast, the flow rate during column loading hardly influenced adsorption efficiency, whereas the temperature and pH value were shown to be crucial parameters determining both total phenolic recovery rates and the adsorption behavior of individual polyphenols. As expected, the eluent composition had the greatest impact on the desorption characteristics of both total and individual phenolic compounds. HPLC analyses revealed significantly different elution profiles of individual polyphenols depending on lipophilicity. This technique allows fractionation of crude plant phenolic extracts, thus providing the opportunity to design the functional properties of the resulting phenolic fractions selectively, and the present study delivers valuable information with regard to the adjustment of individual process parameters.

Novel immunoassay and rapid immunoaffinity chromatography method for the detection and selective extraction of naringin in Citrus aurantium.

PubMed

Qu, Huihua; Zhang, Yue; Qu, Baoping; Cheng, Jinjun; Liu, Shuchen; Feng, Shenglan; Wang, Qingguo; Zhao, Yan

2016-04-01

In this work, a novel monoclonal antibody specific for naringin was prepared and characterized. Subsequently, an indirect competitive enzyme-linked immunosorbent assay for naringin was developed, with an effective range from 4.8 to 156 ng/mL naringin. Next, an immunoaffinity column was obtained by coupling anti-naringin monoclonal antibodies to CNBr-activated Sepharose 4B and a rapid immunoaffinity chromatography assay for naringin was developed. The immunoaffinity column was used to separate naringin from Citrus aurantium. The results showed that 1 g of the dry Sepharose 4B can couple 10 mg of immunoglobulin G. And the immunoaffinity column can efficiently and specifically capture approximately 250 μg of naringin without cross reacting with its structurally similar compounds. Moreover, our results indicate that the application of immunoaffinity chromatography can simplify the pretreatment and the isolation process greatly compared to conventional methods, providing a potential method for extracting the target component from structurally similar compounds in natural products. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Analysis of ethanol-soluble extractives in southern pine wood by low-field proton NMR

Treesearch

Thomas L. Eberhardt; Thomas Elder; Nicole Labbe

2007-01-01

Low-field portion NMR was evaluated as a nondestructive and rapid technique for measuring ethanol-soluble extractives in southern pine wood. Matchstick-sized wood specimens were steeped in extractive-containing solutions to generate extractive-enriched samples for analysis. decay curves obtained by the Carr-Purcell-Meiboom-gill (CPMG) pulse sequence were analyzed with...

Algae as an electron donor promoting sulfate reduction for the bioremediation of acid rock drainage.

PubMed

Ayala-Parra, Pedro; Sierra-Alvarez, Reyes; Field, Jim A

2016-11-05

This study assessed bioremediation of acid rock drainage in simulated permeable reactive barriers (PRB) using algae, Chlorella sorokiniana, as the sole electron donor for sulfate-reducing bacteria. Lipid extracted algae (LEA), the residues of biodiesel production, were compared with whole cell algae (WCA) as an electron donor to promote sulfate-reducing activity. Inoculated columns containing anaerobic granular sludge were fed a synthetic medium containing H2SO4 and Cu(2+). Sulfate, sulfide, Cu(2+) and pH were monitored throughout the experiment of 123d. Cu recovered in the column packing at the end of the experiment was evaluated using sequential extraction. Both WCA and LEA promoted 80% of sulfate removal (12.7mg SO4(2-) d(-1)) enabling near complete Cu removal (>99.5%) and alkalinity generation raising the effluent pH to 6.5. No noteworthy sulfate reduction, alkalinity formation and Cu(2+) removal were observed in the endogenous control. In algae amended-columns, Cu(2+) was precipitated with biogenic H2S produced by sulfate reduction. Formation of CuS was evidenced by sequential extraction and X-ray diffraction. LEA and WCA provided similar levels of electron donor based on the COD balance. The results demonstrate an innovative passive remediation system using residual algae biomass from the biodiesel industry. Copyright © 2016 Elsevier B.V. All rights reserved.

Biodegradable chelate enhances the phytoextraction of copper by Oenothera picensis grown in copper-contaminated acid soils.

PubMed

González, Isabel; Cortes, Amparo; Neaman, Alexander; Rubio, Patricio

2011-07-01

Oenothera picensis plants (Fragrant Evening Primrose) grow in the acid soils contaminated by copper smelting in the coastal region of central Chile. We evaluated the effects of the biodegradable chelate MGDA (methylglycinediacetic acid) on copper extraction by O. picensis and on leaching of copper through the soil profile, using an ex situ experiment with soil columns of varying heights. MGDA was applied in four rates: 0 (control), 2, 6 and 10 mmol plant(-1). MGDA application significantly increased biomass production and foliar concentration, permitting an effective increase in copper extraction, from 0.09 mg plant(-1) in the control, to 1.3mg plant(-1) in the 6 and 10 mmol plant(-1) treatments. With 10 mmol plant(-1) rate of MGDA, the copper concentration in the leachate from the 30 cm columns was 20 times higher than in the control. For the 60 cm columns, copper concentration was 2 times higher than the control. It can be concluded that at increased soil depths, copper leaching would be minimal and that MGDA applications at the studied rates would not pose a high risk for leaching into groundwater. It can thus be stated that applications of MGDA are an effective and environmentally safe way to improve copper extraction by O. picensis in these soils. Copyright © 2011 Elsevier Ltd. All rights reserved.

Simultaneous saccharification and extractive fermentation of lignocellulosic materials into lactic acid in a two-zone fermentor-extractor system.

PubMed

Iyer, P V; Lee, Y Y

1999-01-01

Simultaneous saccharification and extractive fermentation of lignocellulosic materials into lactic acid was investigated using a two-zone bioreactor. The system is composed of an immobilized cell reactor, a separate column reactor containing the lignocellulosic substrate and a hollow-fiber membrane. It is operated by recirculating the cell free enzyme (cellulase) solution from the immobilized cell reactor to the column reactor through the membrane. The enzyme and microbial reactions thus occur at separate locations, yet simultaneously. This design provides flexibility in reactor operation as it allows easy separation of the solid substrate from the microorganism, in situ removal of the product and, if desired, different temperatures in the two reactor sections. This reactor system was tested using pretreated switchgrass as the substrate. It was operated under a fed-batch mode with continuous removal of lactic acid by solvent extraction. The overall lactic acid yield obtainable from this bioreactor system is 77% of the theoretical.

Rapid preconcentration method for the determination of azadirachtin-A and -B, nimbin and salannin in neem oil samples by using graphitised carbon solid phase extraction.

PubMed

Ramesh, A; Balasubramanian, M

1999-01-01

A simple and rapid method involving solid phase extraction and liquid chromatography for the determination of azadirachtin-A and -B, nimbin and salannin at nanogram levels in neem oil samples is presented. The neem oil samples are defatted and the compounds of interest extracted by mixing the sample with hexane and passing the hexane solution through a graphitised carbon black column. After washing the column with 2 ml of hexane, azadirachtin-A and -B, nimbin and salannin are eluted with 5 ml of acetonitrile and quantified using HPLC with UV detection. The recoveries of azadirachtin-A and -B, nimbin and salannin in fortified oil samples were 97.4-104.7%. The upper limit of quantification is up to 100 micrograms ml-1 without any additional clean-up and with little interference from lipids during the analysis by HPLC. The method was successfully applied to various neem oil samples collected from different locations in India.

[HPLC Specific Fingerprint of Alcohol Extract of Andrographis paniculata].

PubMed

Liu, Fei-fei; Fan, Chun-lin; Huang, Xiao-jun; Wang, Gui-yang; Wang, Ying; Ye, Wen-cai

2015-07-01

To establish the specific fingerprint of alcohol extract of Andrographis paniculata by HPLC. The analysis was performed on Cosmosil 5C18 -MS-II (250 mm x 4. 6 mm, 5 µm) column, with gradient phase consisting of acetonitrile and water at the flow rate of 1. 0 mL/min. The UV detection wavelength was set at 225 nm, and column temperature was 30 °C. The specific fingerprint chromatogram was established and seven common peaks were identified by comparison with the reference standards and LC-MS. The relative retention times were 1. 00 (No. 1, andrographolide), 1. 04 (No. 2, deoxyandrographoside), 1. 07 (No. 3, isoandrographolide), 1. 10 (No. 4, 14-deoxy-11, 12-didehydroandrographoside), 1. 50 (No. 5, neoandrographolide), 1. 75 ( No. 6, deoxyandrographolide) and 1. 79 (No. 7, dehydroandrographolide). The method is simple and reproducible with high precision, which can provide the basis for the quality control and evaluation of alcohol extract of Andrographis paniculata and its preparations.

Determination of dioxin-like polychlorinated biphenyls in 1 mL whole blood using programmable temperature vaporization large volume injection coupled to gas chromatogram and high-resolution mass spectrometry.

PubMed

Shen, Haitao; Guan, Rongfa; Li, Jingguang; Zhang, Lei; Ren, Yiping; Xu, Xiaomin; Song, Yang; Zhao, Yunfeng; Han, Jianlong; Wu, Yongning

2013-03-12

A sensitive method based on programmable temperature vaporization large volume injection coupled to gas chromatogram and high-resolution mass spectrometry (PTV-GC-HRMS) has been developed for the determination of ultra trace levels of dioxin-like polychlorinated biphenyls (DL PCBs) in small amounts of human blood. Blood samples (1mL) were first extracted by column extraction and then purified with column chromatorgraphies. Final extracts (20μL) were introduced to the PTV injector under the solvent vent mode and detected by GC-HRMS (SIM mode). PTV parameters were observed by changing one factor at a time (practical conditions: vent flow: 50mLmin(-1), vent pressure: 0kPa and vent time: 0.1min), recoveries of most PCB congeners ranged from 55.1% to 108%, and method detection limits were in the range of 0.11-1.63pgg(-1). Copyright © 2013 Elsevier B.V. All rights reserved.

Isolation, purification, toxicity and some physicochemical properties of mycotoxins produced by aspergillus quadrilineatus isolated from acha (Digitaria exilis stapf) in Plateau State of Nigeria.

PubMed

Gbodi, T A

1993-06-01

Some physico-chemical and toxicological studies were carried out on mycotoxins elaborated by Aspergillus quadrilineatus isolated from a grain foodstuff, acha (Digitaria exilis) in the Plateau State of Nigeria. The mycotoxins produced by A quadrilineatus were extractable from rice culture by chloroform. Column chromatographic separations of the crude extract in silica gel using different elution solvents and biological tests showed that the mycotoxins came off in the diethylether, chloroform and mostly in the ethyl acetate fractions. Use of different available mycotoxin standards on silica gel G coated chromatoplates revealed that 1 of the mycotoxins produced by A quadrilineatus was sterigmatocystin. Two other more toxic mycotoxins were isolated and purified from the crude chloroform extract; their column, preparative thin-layer chromatographic, infrared and UV-spectrophotometric characteristics were established. The infrared spectra of the 2 purified mycotoxins suggested that the carbonyl group of their structures were similar to that of aflatoxin.

Liquid chromatographic determination of acriflavine and proflavine residues in channel catfish muscle.

PubMed

Plakas, S M; el Said, K R; Jester, E L; Bencsath, F A; Hayton, W L

1997-01-01

A liquid chromatographic (LC) method was developed for determination of acriflavine (ACR) and proflavine (PRO) residues in channel catfish muscle. Residues were extracted with acidified methanol solution, and extracts were cleaned up with C18 solid-phase extraction columns. Residue concentrations were determined on an LC cyano column, with spectrophotometric detection at 454 nm. Catfish muscle was individually fortified with ACR (purified from commercial product) and PRO at concentrations of 5, 10, 20, 40, and 80 ppb (5 replicates per level). Mean recoveries from fortified muscle at each level ranged from 86 to 95%, with relative standard deviations (RSDs) of 2.5 to 5.7%. The method was applied to incurred residues of ACR and PRO in muscle after waterborne exposure of channel catfish to commercial acriflavine (10 ppm total dye for 4 h). RSDs for incurred residues of ACR and PRO were in the same range as those for fortified muscle. Low residue concentrations (< 1% of exposure water concentration) suggested poor absorption of ACR and PRO in catfish.

A new linoleiyl arabinopyranoside from the bark of Bauhinia racemosa Lam and a new flavonoidal glycoside from the leaves of Cordia dichotoma Linn.

PubMed

Rahman, Md Azizur; Akhtar, Juber

2016-10-01

Phytochemical investigation is very valuable for the ethnomedicinally important plants Bauhinia racemosa Lam (BR) and Cordia dichotoma Linn (CD) used for the cure of variety of ailments. This study was thus designed for phytochemical investigation of BR bark and CD leaves. Phytoconstituents were isolated from the methanolic extracts of the plants by column chromatography using silica gel as stationary phase. The structures had been established on the basis of their physicochemical and spectral data, i.e. IR, (1)H NMR, (13)C NMR and MS. Elution of the columns with different solvents furnished six compounds (1-6) from the methanolic extract of BR bark and three compounds (7-9) from the methanolic extract of CD leaves which were structurally elucidated. The present phytochemical investigation reported several new compounds useful in increasing the existing knowledge of phytoconstituents from BR bark and CD leaves which is very valuable, as these drugs are used in the Indian traditional systems of medicine.

Affinity monolith-integrated poly(methyl methacrylate) microchips for on-line protein extraction and capillary electrophoresis.

PubMed

Sun, Xiuhua; Yang, Weichun; Pan, Tao; Woolley, Adam T

2008-07-01

Immunoaffinity monolith pretreatment columns have been coupled with capillary electrophoresis separation in poly(methyl methacrylate) (PMMA) microchips. Microdevices were designed with eight reservoirs to enable the electrically controlled transport of selected analytes and solutions to carry out integrated immunoaffinity extraction and electrophoretic separation. The PMMA microdevices were fabricated reproducibly and with high fidelity by solvent imprinting and thermal bonding methods. Monoliths with epoxy groups for antibody immobilization were prepared by direct in situ photopolymerization of glycidyl methacrylate and ethylene glycol dimethacrylate in a porogenic solvent consisting of 70% 1-dodecanol and 30% cyclohexanol. Antifluorescein isothiocyanate was utilized as a model affinity group in the monoliths, and the immobilization process was optimized. A mean elution efficiency of 92% was achieved for the monolith-based extraction of fluorescein isothiocyanate (FITC)-tagged human serum albumin. FITC-tagged proteins were purified from a contaminant protein and then separated electrophoretically using these devices. The developed immunoaffinity column/capillary electrophoresis microdevices show great promise for combining sample pretreatment and separation in biomolecular analysis.

Affinity Monolith-Integrated Poly(methyl Methacrylate) Microchips for On-Line Protein Extraction and Capillary Electrophoresis

PubMed Central

Sun, Xiuhua; Yang, Weichun; Pan, Tao; Woolley, Adam T.

2008-01-01

Immunoaffinity monolith pretreatment columns have been coupled with capillary electrophoresis separation in poly(methyl methacrylate) (PMMA) microchips. Microdevices were designed with 8 reservoirs to enable the electrically controlled transport of selected analytes and solutions to carry out integrated immunoaffinity extraction and electrophoretic separation. The PMMA microdevices were fabricated reproducibly and with high fidelity by solvent imprinting and thermal bonding methods. Monoliths with epoxy groups for antibody immobilization were prepared by direct in-situ photopolymerization of glycidyl methacrylate and ethylene dimethacrylate in a porogenic solvent consisting of 70% dodecanol and 30% hexanol. Anti-fluorescein isothiocyanate (FITC) was utilized as a model affinity group in the monoliths, and the immobilization process was optimized. A mean elution efficiency of 92% was achieved for the monolith-based extraction of FITC-tagged human serum albumin. FITC-tagged proteins were purified from a contaminant protein and then separated electrophoretically using these devices. The developed immunoaffinity column/capillary electrophoresis microdevices show great promise for combining sample pretreatment and separation in biomolecular analysis. PMID:18479142

An HPLC method for determination of azadirachtin residues in bovine muscle.

PubMed

Gai, María Nella; Álvarez, Christian; Venegas, Raúl; Morales, Javier

2011-04-01

A high-performance liquid chromatography (HPLC) method for the determination of azadirachtin (A and B) residues in bovine muscle has been developed. Azadirachtin is a neutral triterpene and chemotherapeutic agent effective in controlling some pest flies in horses, stables, horns and fruit. The actual HPLC method uses an isocratic elution and UV detection. Liquid-liquid extraction and solid-phase purification was used for the clean-up of the biological matrix. The chromatographic determination of these components is achieved using a C18 analytical column with water-acetonitrile mixture (27.5:72.5, v/v) as mobile phase, 1 mL/min as flow rate, 45 °C column temperature and UV detector at 215 nm. The azadirachtin peaks are well resolved and free of interference from matrix components. The extraction and analytical method developed in this work allows the quantitation of azadirachtin with precision and accuracy, establishing a lower limit of quantitation of azadirachtin, extracted from the biological matrix.

Transport and removal of viruses in saturated sand columns under oxic and anoxic conditions--Potential implications for groundwater protection.

PubMed

Frohnert, Anne; Apelt, Susann; Klitzke, Sondra; Chorus, Ingrid; Szewzyk, Regine; Selinka, Hans-Christoph

2014-11-01

To protect groundwater as a drinking water resource from microbiological contamination, protection zones are installed. While travelling through these zones, concentrations of potential pathogens should decline to levels that pose no risks to human health. Removal of viruses during subsurface passage is influenced by physicochemical conditions, such as oxygen concentration, which also affects virus survival. The aim of our study was to evaluate the effect of redox conditions on the removal of viruses during sand filtration. Experiments in glass columns filled with medium-grained sand were conducted to investigate virus removal in the presence and absence of dissolved oxygen. Bacteriophages MS2 and PhiX174, as surrogates for human enteric viruses were spiked in pulsed or in continuous mode and pumped through the columns at a filter velocity of about 1m/d. Virus breakthrough curves were analyzed by calculating total viral elimination and fitted using one-dimensional transport models (CXTFIT and HYDRUS-1D). While short-term experiments with pulsed virus application showed only small differences with regard to virus removal under oxic and anoxic conditions, a long-term experiment with continuous dosing revealed a clearly lower elimination of viruses under anoxic conditions. These findings suggest that less inactivation and less adsorption of viruses in anoxic environments affect their removal. Therefore, in risk assessment studies aimed to secure drinking water resources from viral contamination and optimization of protection zones, the oxic and anoxic conditions in the subsurface should also be considered. Copyright © 2014 Elsevier GmbH. All rights reserved.

Simultaneous determination of nandrolone, testosterone, and methyltestosterone by multi-immunoaffinity column and capillary electrophoresis.

PubMed

Qi, Xiao-Hua; Zhang, Li-Wei; Zhang, Xin-Xiang

2008-08-01

A multitarget antibody immunoaffinity column was proposed for the purification and enrichment of nandrolone, testosterone, and methyltestosterone from urine. Nandrolone-3-site substituted antigen was designed and synthesized and the polyclonal antibody was prepared with immunizing rabbits. The stationary phase of the immunoaffinity column was synthesized by covalently bonding the antibodies specific to nandrolone, testosterone, and methyltestosterone onto CNBr-actived Sepharose 4B. The analytes of interest were extracted with a methanol/water mixture in one step. The immunoaffinity column showed high affinity and high selectivity to a class of structurally related compounds. The elution was then transferred to a micellar electrokinetic CE system with a running buffer of sodium borate and sodium cholate for separation and determination. Recoveries of the three steroids from complex matrix were 88-94% with RSD values less than 5.2%. Optimization of the immunoaffinity column purification was achieved and the feasibility of the technique for the analysis of steroid hormone was discussed. The results indicated that the combination of multi-immunoaffinity column and CE was an effective technique, which was rapid, simple, and sensitive for the assay of steroids.

Changes to the COS Extraction Algorithm for Lifetime Position 3

NASA Astrophysics Data System (ADS)

Proffitt, Charles R.; Bostroem, K. Azalee; Ely, Justin; Foster, Deatrick; Hernandez, Svea; Hodge, Philip; Jedrzejewski, Robert I.; Lockwood, Sean A.; Massa, Derck; Peeples, Molly S.; Oliveira, Cristina M.; Penton, Steven V.; Plesha, Rachel; Roman-Duval, Julia; Sana, Hugues; Sahnow, David J.; Sonnentrucker, Paule; Taylor, Joanna M.

2015-09-01

The COS FUV Detector Lifetime Position 3 (LP3) has been placed only 2.5" below the original lifetime position (LP1). This is sufficiently close to gain-sagged regions at LP1 that a revised extraction algorithm is needed to ensure good spectral quality. We provide an overview of this new "TWOZONE" extraction algorithm, discuss its strengths and limitations, describe new output columns in the X1D files that show the boundaries of the new extraction regions, and provide some advice on how to manually tune the algorithm for specialized applications.

Determination of imidazole derivatives by micellar electrokinetic chromatography combined with solid-phase microextraction using activated carbon-polymer monolith as adsorbent.

PubMed

Shih, Yung-Han; Lirio, Stephen; Li, Chih-Keng; Liu, Wan-Ling; Huang, Hsi-Ya

2016-01-08

In this study, an effective method for the separation of imidazole derivatives 2-methylimidazole (2-MEI), 4- methylimidazole (4-MEI) and 2-acetyl-4-tetrahydroxybutylimidazole (THI) in caramel colors using cation-selective exhaustive injection and sweeping micellar electrokinetic chromatography (CSEI-sweeping-MEKC) was developed. The limits of detection (LOD) and quantitation (LOQ) for the CSEI-sweeping-MEKC method were in the range of 4.3-80μgL(-1) and 14-270μgL(-1), respectively. Meanwhile, a rapid fabrication activated carbon-polymer (AC-polymer) monolithic column as adsorbent for solid-phase microextraction (SPME) of imidazole colors was developed. Under the optimized SPME condition, the extraction recoveries for intra-day, inter-day and column-to-column were in the range of 84.5-95.1% (<6.3% RSDs), 85.6-96.1% (<4.9% RSDs), and 81.3-96.1% (<7.1% RSDs), respectively. The LODs and LOQs of AC-polymer monolithic column combined with CSEI-sweeping-MEKC method were in the range of 33.4-60.4μgL(-1) and 111.7-201.2μgL(-1), respectively. The use of AC-polymer as SPME adsorbent demonstrated the reduction of matrix effect in food samples such as soft drink and alcoholic beverage thereby benefiting successful determination of trace-level caramel colors residues using CSEI-sweeping-MEKC method. The developed AC-polymer monolithic column can be reused for more than 30 times without any significant loss in the extraction recovery for imidazole derivatives. Copyright © 2015 Elsevier B.V. All rights reserved.

Procedure for the determination of retinol and alpha-tocopherol in poultry tissues using capillary gas chromatography with solvent venting injection.

PubMed

Maraschiello, C; García Regueiro, J A

1998-08-28

A procedure designed for the determination of retinol (vitamin A) and alpha-tocopherol (vitamin E) in poultry tissues has been developed. The procedure involves lipid extraction, saponification, solid-phase clean-up and capillary gas chromatography (cGC). Retinol and alpha-tocopherol were determined separately by cGC-flame ionisation detection using a fused-silica open tubular capillary column, 30 m x 0.25 mm I.D. coated with 5% phenylmethylsilicone and with a film thickness of 0.25 micron. Solvent extraction followed by saponification were sufficient to provide a purified extract which was directly analyzed for retinol by cGC in the solvent venting mode. However, in order to accurately determine alpha-tocopherol by cGC, further purification of the extract by solid-phase extraction was necessary. A silica SPE column was used to remove interfering cholesterol from the extract. alpha-Tocopherol was analyzed in its derivatized form. Absolute and relative recoveries for both vitamins from spiked samples were evaluated. Absolute and relative recoveries ranging from 80 to 95% were obtained for both compounds. 5 alpha-Cholestane and alpha-tocopheryl acetate were used as internal standards. Poultry muscle meat and liver tissue were analyzed for their retinol and alpha-tocopherol content and the peaks detected by cGC were confirmed by cGC-mass spectrometry.

Rapid determination of eight bioactive alkaloids in Portulaca oleracea L. by the optimal microwave extraction combined with positive-negative conversion multiple reaction monitor (+/-MRM) technology.

PubMed

Liang, Xiao; Tian, Jinlong; Li, Lingzhi; Gao, Jun; Zhang, Qingyi; Gao, Pinyi; Song, Shaojiang

2014-03-01

A rapid and reliable microwave extraction and the triple quadrupole-linear ion trap mass spectrometry method was developed and validated for the determination of eight alkaloids in Portulaca oleracea L. The optimal microwave extraction (MWE) condition was performed at 60 °C for 12 min with ethanol-water (70:30, v/v) as the extracting solvent, and the solvent to solid ratio was 30:1. The alkaloids were first detected simultaneously by electrospray ionization tandem mass spectrometry under positive-negative conversion multiple reaction monitor ((+/-)MRM) technique. With investigating three different columns, samples were separated in only 8 min on a Waters ACQUITY UPLC HSS T3 (50 × 2.1 mm(2), 1.8 μm) column using acetonitrile and formic acid-water solution as a mobile phase with a flow rate at 0.2 mL/min. All calibration curves showed good linearity (r>0.999) within the test ranges. The method developed was validated with acceptable sensitivity, intra- and inter-day precision, reproducibility, and extraction recoveries. It was successfully applied to the determination of eight alkaloids in Portulaca oleracea L. from different sources and different harvest periods. The method also provide a reference for extraction and determination of alkaloids in other complex systems. © 2013 Elsevier B.V. All rights reserved.

[Studies on technology optimization for extraction and purification of total flavones from root bark of Artocarpus styracifolius].

PubMed

Ren, Gang; Liu, Rong-hua; Shao, Feng; Huang, Hui-lian; Wen, Li-rong

2010-08-01

To study the technology optimization for extraction and purification of total flavones from root bark of Artocarpus styracifolius. The optimum extraction conditions were investigated by the contents of the total flavones, using orthogonal test; Static adsorption capacity and desorption rate were employed as examine items for the screening of optimum macroporous resin and optimum technology for the purification of total flavones with selected macroporous were also investigated. The optimum extraction conditions were as follows: using 60% alcohol of seven times than amounts of original material soaking 12 hours,extracting once with hot reflux method at 50 degrees C. HPD-500 type macroporous resin showed better adsorption and desorption property. The optimum purification conditions were as follows: the sample solution was prepared at the concentration of 50.0 mg/mL, subjected to HPD-500 type macroporous resin column chromatography with a load ratio of 22.0 mg total flavones per gram of resin. After standing for 1 hour, the column was eluted with 4 BV water before being eluted with 4 BV 80% alcohol. The purity of the product was 86.4%, which enhanced the content of total flavones by 533%. The optimum conditions for extraction and purification of total flavones from root bark of Artocarpus styractifolius are convenient and practical, and could be used as a reference for industrial production.

Determination of nonylphenol and nonylphenol ethoxylates in environmental solid samples by ultrasonic-assisted extraction and high performance liquid chromatography-fluorescence detection.

PubMed

Núñez, L; Turiel, E; Tadeo, J L

2007-04-06

A simple and rapid analytical method for the determination of nonylphenol (NP) and nonylphenol ethoxylates (NPEOx) in solid environmental samples has been developed. This method combines an ultrasonic-assisted extraction procedure in small columns and an enrichment step onto C(18) solid-phase extraction cartridges prior to separation using HPLC with fluorescence detection. Method optimization was carried out using soil samples fortified at different concentration levels (from 0.1 to 100 microg/g). Under optimum conditions, 2g of soil was placed in small glass columns and extraction was performed assisted by sonication (SAESC) at 45 degrees C in two consecutive steps of 15 min using a mixture of H(2)O/MeOH (30/70). The obtained extracts were collected, loaded onto 500 mg C(18) cartridges, and analytes were eluted with 3 x 1 ml of methanol and 1 ml of acetonitrile. Finally, sample extracts were evaporated under a nitrogen stream, redissolved in 500 microl H(2)O/AcN (50/50), and passed though a 0.45 microm nylon filter before final determination by HPLC-FL. The developed procedure allowed to achieve quantitative recoveries for NP and NPEOx, and was properly validated. Finally, the method was applied to the determination of these compounds in soils and other environmental solid samples such as sediments, compost and sludge.

DIODE STEERED MANGETIC-CORE MEMORY

DOEpatents

Melmed, A.S.; Shevlin, R.T.; Laupheimer, R.

1962-09-18

A word-arranged magnetic-core memory is designed for use in a digital computer utilizing the reverse or back current property of the semi-conductor diodes to restore the information in the memory after read-out. In order to ob tain a read-out signal from a magnetic core storage unit, it is necessary to change the states of some of the magnetic cores. In order to retain the information in the memory after read-out it is then necessary to provide a means to return the switched cores to their states before read-out. A rewrite driver passes a pulse back through each row of cores in which some switching has taken place. This pulse combines with the reverse current pulses of diodes for each column in which a core is switched during read-out to cause the particular cores to be switched back into their states prior to read-out. (AEC)

Transformation of the ordered internal structures during the acceleration of fast charged particles in a dense plasma focus

NASA Astrophysics Data System (ADS)

Kubes, P.; Paduch, M.; Cikhardt, J.; Cikhardtova, B.; Klir, D.; Kravarik, J.; Rezac, K.; Zielinska, E.; Sadowski, M. J.; Szymaszek, A.; Tomaszewski, K.; Zaloga, D.

2017-07-01

The paper concerns important differences in the evolution of plasma column structures during the production of fusion neutrons in the first and subsequent neutron pulses, as observed for plasma-focus discharges performed with the deuterium filling. The first neutron pulse, of a more isotropic distribution, is usually produced during the formation of the first big plasmoid. The next neutron pulses can be generated by the fast deuterons moving dominantly in the downstream direction, at the instants of a disruption of the pinch constriction, when other plasmoids are formed during the constriction evolution. In both cases, the fusion neutrons are produced by a beam-target mechanism, and the acceleration of fast electron- and deuteron-beams can be interpreted by transformation and decay of the magnetic field associated with a filamentary structure of the current flow in the plasmoid.

Fuel Composition and Performance Analysis of Endothermically Heated Fuels for Pulse Detonation Engines

DTIC Science & Technology

2009-03-01

Waste heat from a pulse detonation engine (PDE) was extracted via concentric, counter flow heat exchangers to produce supercritical pyrolytic...mass spectrometry HLPC = High performance liquid chromatography NPT = National pipe thread PAH = Polycyclic aromatic hydrocarbon PDE = Pulse...Precision Liquid Chromatography (HPLC). The resulting “stressed” fuel showed a 29 shift to lower molecular weight compounds, as well as the production

Role of Noninvasive Hemoglobin Monitoring in Trauma

DTIC Science & Technology

2015-03-25

spectrophotometry-based monitoring technology (Radical-7® Pulse CO- Oximeter ; Masimo Corp., Irvine, CA) that provides continuous hemoglobin...116(1):65-72. 14. Masimo Corp. Radical-7 signal extraction pulse co- oximeter operator’s manual. Irvine (CA): Masimo Corp.; 2007. 15. Bland JM...method similar to conventional pulse oximetry. Transmitted light is captured by photodiode receptor and analyzed to create an analog signal that, in

Recovery of Lithium from Geothermal Brine with Lithium–Aluminum Layered Double Hydroxide Chloride Sorbents

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

Paranthaman, Mariappan Parans; Li, Ling; Luo, Jiaqi

In this paper, we report a three-stage bench-scale column extraction process to selectively extract lithium chloride from geothermal brine. The goal of this research is to develop materials and processing technologies to improve the economics of lithium extraction and production from naturally occurring geothermal and other brines for energy storage applications. A novel sorbent, lithium aluminum layered double hydroxide chloride (LDH), is synthesized and characterized with X-ray powder diffraction, scanning electron microscopy, inductively coupled plasma optical emission spectrometry (ICP-OES), and thermogravimetric analysis. Each cycle of the column extraction process consists of three steps: (1) loading the sorbent with lithium chloridemore » from brine; (2) intermediate washing to remove unwanted ions; (3) final washing for unloading the lithium chloride ions. Our experimental analysis of eluate vs feed concentrations of Li and competing ions demonstrates that our optimized sorbents can achieve a recovery efficiency of ~91% and possess excellent Li apparent selectivity of 47.8 compared to Na ions and 212 compared to K ions, respectively in the brine. Finally, the present work demonstrates that LDH is an effective sorbent for selective extraction of lithium from brines, thus offering the possibility of effective application of lithium salts in lithium-ion batteries leading to a fundamental shift in the lithium supply chain.« less

Semi-industrial isolation of salicin and amygdalin from plant extracts using slow rotary counter-current chromatography.

PubMed

Du, Qizhen; Jerz, Gerold; Ha, Yangchun; Li, Lei; Xu, Yuanjin; Zhang, Qi; Zheng, Qunxiong; Winterhalter, Peterb; Ito, Yoichiro

2005-05-13

Salicin in the bark extract of Salix alba and amygdalin in the fruit extract of Semen armeniacae were each separated by slow rotary counter-current chromatography (SRCCC). The apparatus was equipped with a 40-L column made of 17 mm i.d. convoluted Teflon tubing. A 500g amount of crude extract containing salicin at 13.5% was separated yielding 63.5 g of salicin at 95.3% purity in 20h using methyl tert-butyl ether-l-butanol (1:3) saturated by methanol-water (1:5) as a stationary phase and methanol-water (1:5) saturated by methyl tert-butyl ether-1-butanol (1:3) as a mobile phase. A 400g amount of crude extract containing amygdalin at 55.3% was isolated to yield 221.2g of amygdalin at 94.1% purity in 19h using ethyl acetate-1-butanol (1:2) saturated by water as a stationary phase and water saturated by ethyl acetate-1-butanol (1:2) as a mobile phase. The flow rate of the mobile phase was 50 ml/min. The results show that industrial SRCCC separation of salicin and amygdalin is feasible using a larger column at a higher flow rate of the mobile phase.

Recovery of Lithium from Geothermal Brine with Lithium-Aluminum Layered Double Hydroxide Chloride Sorbents.

PubMed

Paranthaman, Mariappan Parans; Li, Ling; Luo, Jiaqi; Hoke, Thomas; Ucar, Huseyin; Moyer, Bruce A; Harrison, Stephen

2017-11-21

We report a three-stage bench-scale column extraction process to selectively extract lithium chloride from geothermal brine. The goal of this research is to develop materials and processing technologies to improve the economics of lithium extraction and production from naturally occurring geothermal and other brines for energy storage applications. A novel sorbent, lithium aluminum layered double hydroxide chloride (LDH), is synthesized and characterized with X-ray powder diffraction, scanning electron microscopy, inductively coupled plasma optical emission spectrometry (ICP-OES), and thermogravimetric analysis. Each cycle of the column extraction process consists of three steps: (1) loading the sorbent with lithium chloride from brine; (2) intermediate washing to remove unwanted ions; (3) final washing for unloading the lithium chloride ions. Our experimental analysis of eluate vs feed concentrations of Li and competing ions demonstrates that our optimized sorbents can achieve a recovery efficiency of ∼91% and possess excellent Li apparent selectivity of 47.8 compared to Na ions and 212 compared to K ions, respectively in the brine. The present work demonstrates that LDH is an effective sorbent for selective extraction of lithium from brines, thus offering the possibility of effective application of lithium salts in lithium-ion batteries leading to a fundamental shift in the lithium supply chain.

Recovery of Lithium from Geothermal Brine with Lithium–Aluminum Layered Double Hydroxide Chloride Sorbents

DOE PAGES

Paranthaman, Mariappan Parans; Li, Ling; Luo, Jiaqi; ...

2017-10-27

In this paper, we report a three-stage bench-scale column extraction process to selectively extract lithium chloride from geothermal brine. The goal of this research is to develop materials and processing technologies to improve the economics of lithium extraction and production from naturally occurring geothermal and other brines for energy storage applications. A novel sorbent, lithium aluminum layered double hydroxide chloride (LDH), is synthesized and characterized with X-ray powder diffraction, scanning electron microscopy, inductively coupled plasma optical emission spectrometry (ICP-OES), and thermogravimetric analysis. Each cycle of the column extraction process consists of three steps: (1) loading the sorbent with lithium chloridemore » from brine; (2) intermediate washing to remove unwanted ions; (3) final washing for unloading the lithium chloride ions. Our experimental analysis of eluate vs feed concentrations of Li and competing ions demonstrates that our optimized sorbents can achieve a recovery efficiency of ~91% and possess excellent Li apparent selectivity of 47.8 compared to Na ions and 212 compared to K ions, respectively in the brine. Finally, the present work demonstrates that LDH is an effective sorbent for selective extraction of lithium from brines, thus offering the possibility of effective application of lithium salts in lithium-ion batteries leading to a fundamental shift in the lithium supply chain.« less

[Antiinflammatory activity of extracts and fractions obtained from Physalis peruviana L. calyces].

PubMed

Franco, Luis A; Matiz, Germán E; Calle, Jairo; Pinzón, Roberto; Ospina, Luis F

2007-03-01

Cape gooseberry calyces (Physalis peruviana) have been used in folk medicine for their medicinal properties including anticancer, antimycobacterial, antipyretic, diuretic, immunomodulatory and antiinflammatory properties. The antiinflammatory effect was evaluated for extracts and fractions obtained from Physalis peruviana calyces in a mice model of acute inflammation. The fractions responsible for antiinflammatory activity were extracted for possible identification. The Physalis peruviana calyces were extracted by percolation with organic solvents. The primary hydroalcoholic fraction was purified by column chromatography. The antiinflammatory effect of extracts and fractions was evaluated using the 12-O-tetradecanoylphorbol-13-acetate-induced mouse model of ear edema. Thirty-eight secondary fractions were obtained by column chromatography of primary hydroalcoholic fraction. Six fractions, evaluated in 12-O-tetradecanoylphorbol-13-acetate-induced inflammation assay, showed significant antiinflammatory activity (p<0.05). The major fraction, Pp-D28-LF, showed a significant dose-dependent response at doses over 250 microg/ear. The antiinflammatory activity attributed to Physalis peruviana calyces was confirmed and validated its use in folk medicine. Fractions responsible for the antiinflammatory action were identified and seem promising for phytomedicinal development. Further studies are needed to isolate and identify the active constituents of these fractions as well as to ascertain the mechanisms involved in the antiinflammatory effect.

Focused electron and ion beam systems

DOEpatents

Leung, Ka-Ngo; Reijonen, Jani; Persaud, Arun; Ji, Qing; Jiang, Ximan

2004-07-27

An electron beam system is based on a plasma generator in a plasma ion source with an accelerator column. The electrons are extracted from a plasma cathode in a plasma ion source, e.g. a multicusp plasma ion source. The beam can be scanned in both the x and y directions, and the system can be operated with multiple beamlets. A compact focused ion or electron beam system has a plasma ion source and an all-electrostatic beam acceleration and focusing column. The ion source is a small chamber with the plasma produced by radio-frequency (RF) induction discharge. The RF antenna is wound outside the chamber and connected to an RF supply. Ions or electrons can be extracted from the source. A multi-beam system has several sources of different species and an electron beam source.

[Determination of buprofezin, methamidophos, acephate, and triazophos residues in Chinese tea samples by gas chromatography].

PubMed

Zhang, Shuiba; Yi, Jun; Ye, Jianglei; Zheng, Wenhui; Cai, Xueqin; Gong, Zhenbin

2004-03-01

A method has been developed for the simultaneous determination of buprofezin, methamidophos, acephate and triazophos residues in Chinese tea samples. The pesticide residues were extracted from tea samples with a mixture of ethyl acetate and n-hexane (50:50, v/v) at 45 degrees C. The extracts were subsequently treated with a column packed with 40 mg of active carbon by gradient elution with ethyl acetate and n-hexane. Buprofenzin and the three organophosphorus pesticides were analyzed by gas chromatography using a DB-210 capillary column and a nitrogen-phosphorus detector. The recoveries for spiked standards were 73.4%-96.9%. The relative standard deviations were all within 4.63%. The limits of quantitation (3sigma) in the tea samples were about 7.0-12.0 microg/kg.

Determination of N-(trans-4-isopropylcyclohexylcarbonyl)-D-phenylalanine in human plasma by solid-phase extraction and column-switching high-performance liquid chromatography with ultraviolet detection.

PubMed

Ono, I; Matsuda, K; Kanno, S

1996-04-12

A column-switching high-performance liquid chromatography method with ultraviolet detection at 210 nm has been developed for the determination of N-(trans-4-isopropylcyclohexylcarbonyl)-D-phenylalanine (AY4166, I) in human plasma. Plasma samples were prepared by solid-phase extraction with Sep-Pak Light tC18, followed by HPLC. The calibration graph for I was linear in the range 0.1-20 micrograms/ml. The limit of quantitation of I, in plasma, was 0.05 microgram/ml. The recovery of spiked I (0.5 microgram/ml) to drug-free plasma was over 92% and the relative standard deviation of spiked I (0.5 microgram/ml) compared to drug-free plasma was 4.3% (n = 8).

Preliminary extraction of tannins by 1-butyl-3-methylimidazole bromide and its subsequent removal from Galla chinensis extract using macroporous resins.

PubMed

Lu, Chunxia; Luo, Xiaoling; Lu, Liliang; Li, Hongmin; Chen, Xia; Ji, Yong

2013-03-01

In recent years, ionic liquids have become increasingly attractive as 'green solvents' used in the extraction of bioactive compounds from natural plant. However, the separation of ionic liquid from the target compounds was difficult, due to their low vapour pressure and high stabilities. In our study, ionic liquid-based ultrasonic and microwave-assisted extraction was used to obtain the crude tannins, then the macroporous resin adsorption technology was further employed to purify the tannins and remove the ionic liquid from crude extract. The results showed that XDA-6 had higher separation efficiency than other tested resins, and the equilibrium experimental data were well fitted to Langmuir isotherms. Dynamic adsorption and desorption were performed on XDA-6 packed in glass columns to optimise the separation process. The optimum conditions as follows: the ratio of column height to diameter bed was 1:8, flow rate 1 BV/h (bed volume per hour), 85% ethanol was used as eluant while the elution volume was 2 BV. Under the optimised conditions, the adsorption and desoption rate of tannins in XDA-6 were 94.81 and 91.63%, respectively. The content of tannins was increased from 70.24% in Galla chinensis extract to 85.12% with a recovery of 99.06%. The result of ultra-performance liquid chromatography (UPLC)-MS/MS analysis showed that [bmim]Br could be removed from extract. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Critical comparison of the on-line and off-line molecularly imprinted solid-phase extraction of patulin coupled with liquid chromatography.

PubMed

Lhotská, Ivona; Holznerová, Anežka; Solich, Petr; Šatínský, Dalibor

2017-12-01

Reaching trace amounts of mycotoxin contamination requires sensitive and selective analytical tools for their determination. Improving the selectivity of sample pretreatment steps covering new and modern extraction techniques is one way to achieve it. Molecularly imprinted polymers as selective sorbent for extraction undoubtedly meet these criteria. The presented work is focused on the hyphenation of on-line molecularly imprinted solid-phase extraction with a chromatography system using a column-switching approach. Making a critical comparison with a simultaneously developed off-line extraction procedure, evaluation of pros and cons of each method, and determining the reliability of both methods on a real sample analysis were carried out. Both high-performance liquid chromatography methods, using off-line extraction on molecularly imprinted polymer and an on-line column-switching approach, were validated, and the validation results were compared against each other. Although automation leads to significant time savings, fewer human errors, and required no handling of toxic solvents, it reached worse detection limits (15 versus 6 μg/L), worse recovery values (68.3-123.5 versus 81.2-109.9%), and worse efficiency throughout the entire clean-up process in comparison with the off-line extraction method. The difficulties encountered, the compromises made during the optimization of on-line coupling and their critical evaluation are presented in detail. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Antioxidant activity and phenolic compositions of lentil (Lens culinaris var. Morton) extract and its fractions

PubMed Central

Zou, Yanping; Chang, Sam K.C.; Gu, Yan; Qian, Steven Y.

2011-01-01

Phenolic compounds were extracted from Morton lentils using acidified aqueous acetone. The crude Morton extract (CME) was applied onto a macroresin column and desorbed by aqueous methanol to obtain a semi-purified Morton extract (SPME). The SPME was further fractionated over Sephadex LH-20 column into five main fractions (Fr I – Fr V). The phytochemical contents such as total phenolic content (TPC), total flavonoid content (TFC), and condensed tannin content (CTC) of the CME, SPME, and its fractions were examined by colorimetric methods. Antioxidant activity of extracts and fractions were screened by DPPH scavenging activity, trolox equivalent antioxidant capacity (TEAC), ferric reduced antioxidant power (FRAP), and oxygen radical absorbing capacity (ORAC) methods. In addition, the compositions of active fractions were determined by HPLC-DAD and HPLC-MS methods. Results showed that fraction enriched in condensed tannins (Fr V) exhibited significantly higher value of TPC, CTC and higher antioxidant activity as compared to the crude extract, SPME and low-molecular-weight fractions (Fr I – IV). Eighteen compounds existed in those fractions, and seventeen were tentatively identified by UV and MS spectra. HPLC-MS analysis revealed Fr II contained mainly kaempferol glycoside, Fr III and Fr IV mainly contained flavonoid glycosides, and Fr V was composed of condensed tannins. The results suggested that extract of Morton lentils is a promising source of antioxidant phenolics, and may be used as a dietary supplement for health promotion. PMID:21332205

Study of Pulsed vs. RF Plasma Properties for Surface Processing Applications

NASA Astrophysics Data System (ADS)

Tang, Ricky; Hopkins, Matthew; Barnat, Edward; Miller, Paul

2015-09-01

The ability to manipulate the plasma parameters (density, E/N) was previously demonstrated using a double-pulsed column discharge. Experiments extending this to large-surface plasmas of interest to the plasma processing community were conducted. Differences between an audio-frequency pulsed plasma and a radio-frequency (rf) discharge, both prevalent in plasma processing applications, were studied. Optical emission spectroscopy shows higher-intensity emission in the UV/visible range for the pulsed plasma comparing to the rf plasma at comparable powers. Data suggest that the electron energy is higher for the pulsed plasma leading to higher ionization, resulting in increased ion density and ion flux. Diode laser absorption measurements of the concentration of the 1S5 metastable and 1S4 resonance states of argon (correlated with the plasma E/N) provide comparisons between the excitation/ionization states of the two plasmas. Preliminary modeling efforts suggest that the low-frequency polarity switch causes a much more abrupt potential variation to support interesting transport phenomena, generating a ``wave'' of higher temperature electrons leading to more ionization, as well as ``sheath capture'' of a higher density bolus of ions that are then accelerated during polarity switch.

Utilizing a library of synthetic affinity ligands for the enrichment, depletion and one-step purification of leech proteins.

PubMed

Dong, Dexian; Gui, Yanli; Chen, Dezhao; Li, Rongxiu

2008-01-01

Although the concept of affinity purification using synthetic ligands had been utilized for many years, there are few articles related to this research area, and they focus only on the affinity purification of specific protein by a defined library of synthetic ligands. This study presents the design and construction of a 700-member library of synthetic ligands in detail. We selected 297 ligand columns from a 700-member library of synthetic ligands to screen leech protein extract. Of the 297, 154 columns had an enrichment effect, 83 columns had a depletion effect, 36 columns had a one-step purification effect, and 58 columns had a one-step purification via flowthrough effect. The experimental results achieved by this large library of affinity ligands provide solid convincing data for the theory that affinity chromatography could be used for the enrichment of proteins that are present in low abundance, the depletion of high abundance proteins, and one-step purification of special proteins. 2008 John Wiley & Sons, Ltd

Supramolecular Affinity Chromatography for Methylation-Targeted Proteomics.

PubMed

Garnett, Graham A E; Starke, Melissa J; Shaurya, Alok; Li, Janessa; Hof, Fraser

2016-04-05

Proteome-wide studies of post-translationally methylated species using mass spectrometry are complicated by high sample diversity, competition for ionization among peptides, and mass redundancies. Antibody-based enrichment has powered methylation proteomics until now, but the reliability, pan-specificity, polyclonal nature, and stability of the available pan-specific antibodies are problematic and do not provide a standard, reliable platform for investigators. We have invented an anionic supramolecular host that can form host-guest complexes selectively with methyllysine-containing peptides and used it to create a methylysine-affinity column. The column resolves peptides on the basis of methylation-a feat impossible with a comparable commercial cation-exchange column. A proteolyzed nuclear extract was separated on the methyl-affinity column prior to standard proteomics analysis. This experiment demonstrates that such chemical methyl-affinity columns are capable of enriching and improving the analysis of methyllysine residues from complex protein mixtures. We discuss the importance of this advance in the context of biomolecule-driven enrichment methods.

Mini-column assay for rapid detection of malachite green in fish.

PubMed

Shalaby, Ali R; Emam, Wafaa H; Anwar, Mervat M

2017-07-01

A simple, rapid and economical mini-column method for detecting malachite green (MG) residue in fish was developed. The method used a column with 2mm ID that was tightly packed with silica gel followed by alumina. Detection of MG was performed by viewing the developed mini-column at visible light by naked eye; where MG was seen as compact green band at the confluence of the silica gel layer with alumina layer. The limit of detection of the assay was 2ng which conform the minimum required performance limit (MRPL). Evaluation utility of the method indicated that all blank and spiked samples at levels below MRPL were assessed as accepted. The intensity of the green band increased whenever MG level in the extract increased; indicated that suggested mini-column technique could be used for semi-quantitative determination of MG in fish samples. The method can be used to select the questionable samples. Copyright © 2017 Elsevier Ltd. All rights reserved.

A green strategy for desorption of trihalomethanes adsorbed by humin and reuse of the fixed bed column.

PubMed

Cunha, G C; Romão, L P C; Santos, M C; Costa, A S; Alexandre, M R

2012-03-30

The objective of the present work was to develop a thermal desorption method for the removal of trihalomethanes (THM) adsorbed by humin, followed by multiple recycling of the fixed bed column in order to avoid excessive consumption of materials and reduce operating costs. The results obtained for adsorption on a fixed bed column confirmed the effectiveness of humin as an adsorbent, extracting between 45.9% and 90.1% of the total THM (TTHM). In none of the tests was the column fully saturated after 10h. Experiments involving thermal desorption were used to evaluate the potential of the technique for column regeneration. The adsorptive capacity of the humin bed increased significantly (p<0.05) between the first and fifth desorption cycle, by 18.9%, 18.1%, 24.2%, 20.2% and 24.2% for CHBr(3), CHBr(2)Cl, CHBrCl(2), CHCl(3) and TTHM, respectively. Copyright © 2011 Elsevier B.V. All rights reserved.

The Identification of a Legionella pneumophila Toxin with in vivo Lethality

DTIC Science & Technology

1980-01-01

It lacked hydroxy fatty a similar extract, obtained from a newly acids , was minimally inhibited by treat- discovered, but genetically unrelated, ment...applied to the Molecular Weight Estimation column depending upon the individual acid supernatant preparation. There A Sephadex G-50 column (1.5 x...Table 1). Although 0.5 ml of the first peak readi- One-milligram amounts of protein ly kills mice within 18 hours, as much as from Legionella acid

Simultaneous Extraction of Lithium and Hydrogen from Seawater

DTIC Science & Technology

2011-04-26

chromatography . Anions were analyzed by Anion Ion Chromatography (Instrument Dionex ICS-1500, Column Dionex AS9-HC; AG9-HC Guard, eluent: 9.00 mM Na2CO3, flow...rate: 1.25 mL/min, and sample loop was 25 μL). Cations were analyzed by Cation Ion Chromatography (Instrument Dionex DX-500, Cation Column Dionex ...the amount was measured volumetrically. Ion chromatography : Ions in seawater diffused from/to the anode and cathode were determined by ion

Liquid chromatographic determination of microcystins in water samples following pre-column excimer fluorescence derivatization with 4-(1-pyrene)butanoic acid hydrazide.

PubMed

Hayama, Tadashi; Katoh, Kenji; Aoki, Takayoshi; Itoyama, Miki; Todoroki, Kenichiro; Yoshida, Hideyuki; Yamaguchi, Masatoshi; Nohta, Hitoshi

2012-11-28

A method to measure the concentrations of microcystins (MCs) in water samples has been developed by incorporating pre-column fluorescence derivatization and liquid chromatography (LC). A solid-phase extraction for pretreatment was used to extract the MCs in water samples. The MCs were derivatized with excimer-forming 4-(1-pyrene)butanoic acid hydrazide (PBH). The MCs could then be detected by fluorescence after separation with a pentafluorophenyl (PFP)-modified superficially porous (core shell) particle LC column. The derivatization reactions of MCs with PBH proceeded easily in the presence of 4,6-dimethoxy-1,3,5-triazin-2-yl-4-methylmorpholinium (DMT-MM) as a condensation reagent, and the resulting derivatives could be easily separated on the PFP column. The derivatives were selectively detected at excimer fluorescence wavelengths (440-540 nm). The instrument detection limit and the instrument quantification limit of the MCs standards were 0.4-1.2 μg L(-1) and 1.4-3.9 μg L(-1), respectively. The method was validated at 0.1 and 1.0 μg L(-1) levels in tap and pond water samples, and the recovery of MCs was between 67 and 101% with a relative standard deviation of 11%. The proposed method can be used to quantify trace amounts of MCs in water samples. Copyright © 2012 Elsevier B.V. All rights reserved.

The Perils of Pathogen Discovery: Origin of a Novel Parvovirus-Like Hybrid Genome Traced to Nucleic Acid Extraction Spin Columns

PubMed Central

Naccache, Samia N.; Greninger, Alexander L.; Lee, Deanna; Coffey, Lark L.; Phan, Tung; Rein-Weston, Annie; Aronsohn, Andrew; Hackett, John; Delwart, Eric L.

2013-01-01

Next-generation sequencing was used for discovery and de novo assembly of a novel, highly divergent DNA virus at the interface between the Parvoviridae and Circoviridae. The virus, provisionally named parvovirus-like hybrid virus (PHV), is nearly identical by sequence to another DNA virus, NIH-CQV, previously detected in Chinese patients with seronegative (non-A-E) hepatitis. Although we initially detected PHV in a wide range of clinical samples, with all strains sharing ∼99% nucleotide and amino acid identity with each other and with NIH-CQV, the exact origin of the virus was eventually traced to contaminated silica-binding spin columns used for nucleic acid extraction. Definitive confirmation of the origin of PHV, and presumably NIH-CQV, was obtained by in-depth analyses of water eluted through contaminated spin columns. Analysis of environmental metagenome libraries detected PHV sequences in coastal marine waters of North America, suggesting that a potential association between PHV and diatoms (algae) that generate the silica matrix used in the spin columns may have resulted in inadvertent viral contamination during manufacture. The confirmation of PHV/NIH-CQV as laboratory reagent contaminants and not bona fide infectious agents of humans underscores the rigorous approach needed to establish the validity of new viral genomes discovered by next-generation sequencing. PMID:24027301

Initiation of insensitive explosives by laser energy

NASA Technical Reports Server (NTRS)

Menichelli, V. J.; Yang, L. C.

1972-01-01

Instantaneous longitudinal detonations were observed in confined columns of pentaerythritol tetranitrate (PETN), cyclotrimethylene trinitramine (RDX), and tetryl when these materials were pulsed with light energy from a focused Q-switch ruby laser. The laser energy ranged from 0.5 to 4.2 J with a pulse width of 25 ns. Enhancement of the ignition mechanism is hypothesized when a 100-nm (1000-A) thick aluminum film is vacuum-deposited on the explosive side of the window. Upon irradiation from the laser, a shock is generated at the aluminum explosive interface. Steady state detonations can be reached in less than 0.5 microseconds with less than 10% variation in detonation velocity for PETN and RDX.

Display system employing acousto-optic tunable filter

NASA Technical Reports Server (NTRS)

Lambert, James L. (Inventor)

1995-01-01

An acousto-optic tunable filter (AOTF) is employed to generate a display by driving the AOTF with a RF electrical signal comprising modulated red, green, and blue video scan line signals and scanning the AOTF with a linearly polarized, pulsed light beam, resulting in encoding of color video columns (scan lines) of an input video image into vertical columns of the AOTF output beam. The AOTF is illuminated periodically as each acoustically-encoded scan line fills the cell aperture of the AOTF. A polarizing beam splitter removes the unused first order beam component of the AOTF output and, if desired, overlays a real world scene on the output plane. Resolutions as high as 30,000 lines are possible, providing holographic display capability.

Display system employing acousto-optic tunable filter

NASA Technical Reports Server (NTRS)

Lambert, James L. (Inventor)

1993-01-01

An acousto-optic tunable filter (AOTF) is employed to generate a display by driving the AOTF with a RF electrical signal comprising modulated red, green, and blue video scan line signals and scanning the AOTF with a linearly polarized, pulsed light beam, resulting in encoding of color video columns (scan lines) of an input video image into vertical columns of the AOTF output beam. The AOTF is illuminated periodically as each acoustically-encoded scan line fills the cell aperture of the AOTF. A polarizing beam splitter removes the unused first order beam component of the AOTF output and, if desired, overlays a real world scene on the output plane. Resolutions as high as 30,000 lines are possible, providing holographic display capability.

Sample injector for high pressure liquid chromatography

DOEpatents

Paul, Phillip H.; Arnold, Don W.; Neyer, David W.

2001-01-01

Apparatus and method for driving a sample, having a well-defined volume, under pressure into a chromatography column. A conventional high pressure sampling valve is replaced by a sample injector composed of a pair of injector components connected in series to a common junction. The injector components are containers of porous dielectric material constructed so as to provide for electroosmotic flow of a sample into the junction. At an appropriate time, a pressure pulse from a high pressure source, that can be an electrokinetic pump, connected to the common junction, drives a portion of the sample, whose size is determined by the dead volume of the common junction, into the chromatographic column for subsequent separation and analysis. The apparatus can be fabricated on a substrate for microanalytical applications.

SEMG-controlled telephone interface for people with disabilities.

PubMed

Chen, Yu-Luen; Lai, Jin-Shin; Luh, Jer-Junn; Kuo, Te-Son

2002-01-01

This paper proposes the development of a surface electromyographic (SEMG)-controlled telephone interface for the disabled. The system is composed of three major components: (1) a SEMG receiving/signal-processing module; (2) a row-column scanning interface for the telephone dialling pad; and (3) a main controller, the Intel-8951 microprocessor. The design concept was based on the idea of using a SEMG generated by the disabled and converting it into a trigger pulse. This could allow convenient control of the dialing motion in the row-column scanning keys of a telephone dialling pad. People with disabilities are competent for certain kinds of work such as being a telephone operator. The increase of opportunities to perform a job for the disabled would help them live independently.

Simultaneous UPLC-MS/MS analysis of native catechins and procyanidins and their microbial metabolites in intestinal contents and tissues of male Wistar Furth inbred rats.

PubMed

Goodrich, Katheryn M; Neilson, Andrew P

2014-05-01

Procyanidins have been extensively investigated for their potential health protective activities. However, the potential bioactivities of procyanidins are limited by their poor bioavailability. The majority of the ingested dose remains unabsorbed and reaches the colon where extensive microbial metabolism occurs. Most existing analytical methods measure either native compounds (catechins and procyanidins), or their microbial metabolites. The objectives of this study were to develop a high-throughput extraction and UPLC-MS/MS method for simultaneous measurement of both native procyanidins and their metabolites, facilitating high-throughput analysis of native and metabolite profiles in various regions of the colon. The present UPLC-MS/MS method facilitates simultaneous resolution and detection of authentic standards of 14 native catechin monomers and procyanidins, as well as 24 microbial metabolites. Detection and resolution of an additional 3 procyanidin dimers and 10 metabolites for which standards were not available was achieved. Elution and adequate resolution of both native compounds and metabolites were achieved within 10min. The intraday repeatability for native compounds was between 1.1 and 16.5%, and the interday repeatability for native compounds was between 2.2 and 25%. Intraday and interday repeatability for metabolites was between 0.6 and 24.1% and 1 and 23.9%, respectively. Observed lower limits of quantification for native compounds were ∼9-350fmol on-column, and for the microbial metabolites were ∼0.8-12,000fmol on-column. Observed lower limits of detection for native compounds were ∼4.5-190fmol on-column, and for metabolites were 0.304-6020fmol on-column. For native monomers and procyanidins, extraction recoveries ranged from 38 to 102%. Extraction recoveries for the 9 microbial metabolites tested ranged from 41 to 95%. Data from tissue analysis of rats gavaged with grape seed extract indicate fairly high accumulation of native compounds, primarily monomers and dimers, in the cecum and colon. Metabolite data indicate the progressive nature of microbial metabolism as the digesta moves through the lower GI tract. This method facilitates the high-throughput, sensitive, and simultaneous analysis of both native compounds and their microbial metabolites in biological samples and provides a more efficient means of extraction and analysis than previous methods. Copyright © 2014 Elsevier B.V. All rights reserved.