WorldWideScience

Sample records for bead-injection lab-on-valve hyphenated

  1. On-line dynamic extraction and automated determination of readily bioavailable hexavalent chromium in solid substrates using micro-sequential injection bead-injection lab-on-valve hyphenated with electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Long, Xiangbao; Miró, Manuel; Hansen, Elo Harald

    2006-01-01

    A novel and miniaturized micro-sequential injection bead injection lab-on-valve (μSI-BI-LOV) fractionation system was developed for in-line microcolumn soil extraction under simulated environmental scenarios and accurate monitoring of the content of easily mobilisable hexavalent chromium in soil ...

  2. Hyphenating multisyringe flow injection lab-on-valve analysis with atomic fluorescence spectrometry for on-line bead injection preconcentration and determination of trace levels of hydride-forming elements in environmental samples.

    Science.gov (United States)

    Long, Xiangbao; Miró, Manuel; Hansen, Elo Harald; Estela, José Manuel; Cerdà, Víctor

    2006-12-15

    In this work the third generation of flow injection analysis, that is, the so-called micro-lab-on-valve (microLOV) approach, is proposed for the first time for the separation, preconcentration, and monitoring of metalloids as hyphenated with atomic fluorescence spectrometry (AFS). This was made feasible by interfacing the micromachined LOV-module with AFS by a multisyringe flowing stream network for on-line postcolumn derivatization of the eluate aimed at generation of hydride species. The potential of this new hyphenated technique for environmental assays was ascertained via determination of ultratrace level concentrations of total inorganic arsenic in freshwater. Employing quantitative preoxidation of As(III) to As(V) in the samples by means of permanganate, the method involves preconcentration of arsenate at pH 10 on a renewable anion exchanger, namely, Q-Sepharose, packed in a LOV microcolumn. The analyte species is afterward stripped out and concurrently prereduced by a 300 microL eluent plug containing 6 mol L(-)1 HCl and 10% KI. The eluate is downstream merged with a metered volume of sodium tetrahydroborate (0.3% w/v) for generation of arsine, which is subsequently quantified by AFS. The flow system facilitates on-column reduction of the retained arsenic with no need for application of programmable stopped flow. Yet, the high concentration of reductant and extreme pH conditions for elution hinder the sorbent to be reused due to gradual deactivation of the functional moieties, so that maximum benefit can be taken from the application of the bead renewable strategy. The proposed procedure is characterized by a high tolerance to metal species and interfering hydride-forming elements. In fact, ratios of Se(IV) to As < or = 5000 and Sb(V) to As < or = 500 are tolerated at the 10% interference level. Under the optimized experimental conditions, a detection limit (3sigma) of 0.02 ng mL(-1) As, a dynamic linear range of 0.05-2.0 ng mL(-1) As (by tailoring the AFS

  3. Hyphenating multisyringe flow injection lab-on-valve analysis with atomic fluorescence spectrometry for on-line bead-injection preconcentration and determination of trace levels of hydride-forming elements in environmental samples

    DEFF Research Database (Denmark)

    Long, Xiangbao; Miró, Manuel; Hansen, Elo Harald;

    2006-01-01

    In this work, the third generation of flow injection analysis, that is, the so-called micro-Lab-on-Valve (μLOV) approach, is proposed for the first time for the separation, preconcentration and monitoring of metalloids as hyphenated with atomic fluorescence spectrometry (AFS). This was made...... feasible by interfacing the micromachined LOV-module with AFS by a multisyringe flowing stream network for on-line post column derivatization of the eluate aimed at the generation of hydride species. The potential of this new hyphenated technique for environmental assays was ascertained via...... quantified by AFS. The flow system facilitates on-column reduction of the retained arsenic with no need for application of programmable stopped-flow. Yet, the high concentration of reductant and extreme pH conditions for elution hinder the sorbent to be re-used due to the gradual deactivation...

  4. Universal approach for selective trace metal determinations via sequential injection-bead injection-lab-on-valve using renewable hydrophobic bead surfaces as reagent carriers

    DEFF Research Database (Denmark)

    Long, Xiangbao; Miró, Manuel; Hansen, Elo Harald

    2005-01-01

    A new concept is presented for selective and sensitive determination of trace metals via electrothermal atomic absorption spectrometry (ETAAS) based on the principle of bead injection (BI) with renewable reversed-phase surfaces in a sequential injection-lab-on-valve (SI-LOV) mode. The methodology...... involves the use of poly(styrene-divinylbenzene) beads containing pendant octadecyl moieties (C18-PS/DVB), which are preimpregnated with a selective organic metal chelating agent prior to the automatic manipulation of the beads in the microbore conduits of the LOV unit. By adapting this approach, the...... immobilization of the most suitable chelating agent can be effected irrespective of the kinetics involved, optimal reaction conditions can be used for implementing the chelating reaction of the target metal analyte with the immobilized reagent, and an added degree of freedom is offered in selecting the most...

  5. Bead Injection Extraction Chromatography using High-capacity Lab-on-Valve as a Front End to Inductively Coupled Plasma Mass Spectrometry for Rapid Urine Radiobioassay

    DEFF Research Database (Denmark)

    Qiao, Jixin; Hou, Xiaolin; Roos, Per;

    2013-01-01

    A novel bead injection (BI) extraction chromatographic microflow system exploiting high-capacity lab-on-valve (LOV) platform coupled with inductively coupled plasma mass spectrometric detection is developed for rapid and automated determination of plutonium in human urine. A microconduit (1 m......L) incorporated within the LOV processing unit is loaded on-line with a metered amount of disposable extraction chromatographic resin (up to 330 mg of TEVA) through programmable beads transport. Selective capture and purification of plutonium onto the resin beads is then performed by pressure driven flow after.......319 ± 0.004 g, n=5). The chemical yields of plutonium were averagely better than 90% under the optimal experimental conditions and the entire analytical procedure could be accomplished within a short timeframe (

  6. Sequential injection/bead injection lab-on-valve schemes for on-line solid phase extraction and preconcentration of ultra-trace levels of heavy metals with determination by ETAAS and ICPMS

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald; Miró, Manuel

    2003-01-01

    This communication presents an overview of the state-of-the-art of the exploitation of sequential injection (SI)-bead injection (BI)-lab-on-valve (LOV) schemes for automatic on-line sample pre-treatments interfaced with ETAAS and ICPMS detection as conducted in the authors' group. The discussions...... are focused on the applications of SI-BI-LOV protocols for on-line microcolumn based solid phase extraction of ultra-trace levels of heavy metals, employing the so-called renewable surface separation and preconcentration manipulatory scheme. Two types of sorbents have been employed as packing material...

  7. Multisyringe flow injection lab-on-valve systems coupled to hydride generation atomic fluorescence spectrometry for on-line bead-injection preconcentration and determination of total inorganic arsenic in environmental waters

    DEFF Research Database (Denmark)

    Long, Xiangbao; Miró, Manuel; Hansen, Elo Harald;

    In this work, the third generation of flow injection analysis, that is, the so-called micro-Lab-on-Valve (LOV) approach, is hyphenated for the first time to atomic fluorescence spectrometry (AFS) for the separation, preconcentration and monitoring of hydride forming elements. A multisyringe flowing...... before loading into the multisyringe flow system. The flow system facilitates on-column reduction with no need for application of programmable stopped-flow. Yet, the high electrolyte concentrations and extreme pH conditions for elution prevents the sorbent to be re-used, so that maximum benefit can...

  8. A Universal Approach for Selective Trace Metal Determinations via Sequential Injection-Bead Injection-Lab-on-Valve (SI-BI-LOV) Using Renewable Reagent-loaded Hydrophobic Beads

    DEFF Research Database (Denmark)

    Long, Xiangbao; Miró, Manuel; Hansen, Elo Harald

    A new sample pretreatment approach is presented for selective and sensitive determination of trace metals via electrothermal atomic absorption spectrometry (ETAAS) based on the principle of bead injection (BI) with renewable reagent-loaded hydrophobic beads in a Sequential Injection-Lab-on-Valve ......A new sample pretreatment approach is presented for selective and sensitive determination of trace metals via electrothermal atomic absorption spectrometry (ETAAS) based on the principle of bead injection (BI) with renewable reagent-loaded hydrophobic beads in a Sequential Injection...... that the bead material can endure very high acidity which is a prerequisite for the reaction. On-line sample pH adjustment prevents alteration of the original distribution of the chromium species, while assuring fast rates for the DPC-Cr(VI) reaction. The proposed procedure was successfully applied...... for the determination of trace levels of Cr(VI) in natural waters of variable cpmpexity. Furthermore, it was validated by the determination of total chromium in a NIST standard reference material (NIST 1640, natural water) after Cr(III) oxidation....

  9. Sequential injection-bead injection-lab-on-valve schemes for on-line solid phase extraction and preconcentration of ultra-trace levels of heavy metals with determination by electrothermal atomic absorption spectrometry and inductively coupled plasma mass spectrometry

    International Nuclear Information System (INIS)

    This communication presents an overview of the state-of-the-art of the exploitation of sequential injection (SI)-bead injection (BI)-lab-on-valve (LOV) schemes for automatic on-line sample pre-treatments interfaced with ETAAS and ICPMS detection as conducted in the authors' group. The discussions are focused on the applications of SI-BI-LOV protocols for on-line microcolumn based solid phase extraction of ultra-trace levels of heavy metals, employing the so-called renewable surface separation and preconcentration manipulatory scheme. Two types of sorbents have been employed as packing material, that is, the hydrophilic SP Sephadex C-25 cation exchange and iminodiacetate based Muromac A-1 chelating resins, and the hydrophobic poly(tetrafluoroethylene) (PTFE) and poly(styrene-divinylbenzene) copolymer alkylated with octadecyl groups (C18-PS/DVB). Using ETAAS as detection device, the easy-to-handle hydrophilic renewable reactors hold the features of improved R.S.D.s and LODs as compared to those operated in the conventional, permanent mode, in addition to the elimination of flow resistance. The hydrophobic columns fall into two categories, that is, the renewable one packed with C18-PS/DVB beads entails analogous R.S.D.s and LODs with respect to the conventional approach, while those with PTFE beads result in slightly inferior R.S.D.s and LODs by similar comparison, yet offering a wider dynamic range than when using an external permanent column. Moreover, the hydrophilic materials result in much higher enrichment of the analyte than the hydrophobic ones, although PTFE is the packing material that exhibits the best retention efficiency

  10. Exploiting the bead-injection approach in the integrated sequential injection Lab-on-Valve format using hydrophobic packing materials for on-line matrix removal and preconcentration of trace levels of cadmium in environmental and biological samples via formation of non-charged chelates prior

    DEFF Research Database (Denmark)

    Miró, Manuel; Jonczyk, Sylwia; Wang, Jianhua;

    2003-01-01

    The concept of renewable microcolumns within the conduits of an automated single injection lab-on-valve system was exploited in a sorption/elution fashion using sorbents of hydrophobic nature. The scheme's practical applicability was demonstrated for the electrothermal atomic absorption spectrome...

  11. On-line dynamic extraction and automated determination of readily bioavailable hexavalent chromium in solid substrates using micro-sequential injection bead-injection lab-on-valve hyphenated with electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Long, Xiangbao; Miró, Manuel; Hansen, Elo Harald

    2006-01-01

    ). The effect of simulated acidic rain on the accessibility of chromate forms for plant uptake was also investigated. The proposed approach offers several advantages over conventional speciation/fractionation protocols in the batch mode, including immediate separation with concomitant preconcentration of...

  12. Fully automated lab-on-valve-multisyringe flow injection analysis-ICP-MS system: An effective tool for fast, sensitive and selective determination of thorium and uranium at environmental levels exploiting solid phase extraction

    OpenAIRE

    Avivar, Jessica; Ferrer, Laura; Casas, Montserrat; Cerdà, Víctor

    2012-01-01

    An on-line solid-phase extraction method linked to inductively coupled mass spectrometry (ICP-MS) has been developed for the determination of low levels of uranium and thorium in environmental samples. The hyphenation of lab-on-valve (LOV) and multisyringe flow injection analysis (MSFIA), coupled to an ICP-MS, allows the simultaneous determination of thorium and uranium in different types of environmental sample matrices achieving high selectivity and sensitivity levels. On-line separation an...

  13. Sequential injection lab-on-valve: the third generation of flow injection analysis

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2003-01-01

    Termed the third generation of flow injection analysis, sequential injection (SI)-lab-on-valve (LOV) has specific advantages and allows novel, unique applications - not least as a versatile front end to a variety of detection techniques. This review presents snd discusses progress to date of the SI...

  14. Universal approach for selective trace metal determinations via sequential injection-bead injection-lab-on-valve using renewable hydrophobic bead surfaces as reagent carriers

    DEFF Research Database (Denmark)

    Long, Xiangbao; Miró, Manuel; Hansen, Elo Harald

    2005-01-01

    that the bead material exhibits excellent chemical stability at low pH values. On-line pH sample adjustment prevents alteration of the original distribution of chromium species while assuring fast rates for the DPC-Cr(VI) reaction. The proposed procedure was successfully applied to the determination of trace...... levels of Cr(VI) in natural waters containing high levels of dissolved salts (such as seawater and hard tap water) without requiring any dilution step. Method validation was performed by determination of total chromium in an NIST standard reference material (NIST 1640, natural water) after Cr...

  15. New Trends in Flow Injection Analysis: Exploitation of Sequential and Lab-on-Valve Schemes

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    Over the past 25 years, Flow Injection Analysis (FIA) has established itself as an indispensable analytical concept that not only has permitted the implementation of numerous intriguing analysis procedures. But, more importantly, it has made it possible to facilitate the execution of procedures...... has appeared, that is, the Lab-on-Valve (LOV) approach, the conceptual basis of which is to incorporate all the necessary unit operational manipulations required, and, when possible, even the detection device into a single small integrated microconduit, or “laboratory”, placed atop a selection valve...

  16. Determination of Low Level Concentrations of Metals by Means of Sequential Injection (SI) and Lab-on-Valve (LOV) Methodologies

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Miró, Manuel; Petersen, Roongrat

    In recent years sequential injection (SI) analysis and Lab-on-Valve (LOV) approaches have proven themselves as powerful and versatile front ends to implement suitable pre-treatment procedures (separation and pre-concentration) for the assay of low concentrations of metals, as amply reflected...... of environmental interest as demonstrated by the accommodation of both single and sequential extraction schemes for metal fractionation of solid samples of environmental concern (e.g. soils and sediments) packed within dedicated microcartridges. An account of the construction and the experimental modes of operandi...

  17. Determination of Low Level Concentrations of Metals by Means of Sequential Injection (SI) and Lab-on-Valve (LOV) Methodologies

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    In recent years sequential injection (SI) analysis and Lab-on-Valve (LOV) approaches have proven themselves as powerful and versatile front ends to implement suitable pre-treatment procedures (separation and pre-concentration) for the assay of low concentrations of metals, as amply reflected...... packed with suitable materials, the emphasis in this lecture will be on applying solid-phase extraction in the SI/LOV mode. Providing unique characteristics and specific advantages, particularly allowing to take advantage of the so-called renewable approach, where the solid-phase material, if called for...... to handle solid samples of environmental interest as demonstrated by the accommodation of both single and sequential extraction schemes for metal fractionation of solid samples of environmental concern (e.g. soils and sediments) packed within dedicated microcartridges. A brief account of the construction...

  18. Interfacing microfluidic handling with spectroscopic detection for real-life applications via the lab-on-valve platform: A review

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Miró, Manuel

    2008-01-01

    with syringe pump propelling devices as a front end to a plethora of spectroscopic detection schemes including UV-Vis spectroscopy, spectrofluorimetry, chemiluminescence, AAS, AFS and ICP-AES/MS. In contrast to lab-on-a-chip units, the versatile configuration of the micromachined LOV readily facilitates...... the implementation of on-line unit operations at will encompassing not merely the introduction of minute, well-defined volumes of sample followed by chemical derivatization, but the potential for accommodation of solid-phase extraction, hydride/vapour generation, precipitation/coprecipitation and bead injection...

  19. Extraction and preconcentration of trace levels of cobalt using functionalized magnetic nanoparticles in a sequential injection lab-on-valve system with detection by electrothermal atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Graphical abstract: An approach to performing extraction and preconcentration employing functionalized magnetic particles for the determination of cobalt in the sequential injection lab-on-valve system using detection by electrothermal atomic absorption spectrometry. Highlights: ► New SPE method for cobalt separation/preconcentration was reported. ► Functionalized magnetic nanoparticles were used as adsorbent. ► Extraction, elution, and detection procedures were performed in the LOV system. ► This automatic extraction technique provided a good platform for metal analysis. - Abstract: A new approach to performing extraction and preconcentration employing functionalized magnetic nanoparticles for the determination of trace metals is presented. Alumina-coated iron oxide nanoparticles were synthesized and used as the solid support. The nanoparticles were functionalized with sodium dodecyl sulfate and used as adsorbents for solid phase extraction of the analyte. Extraction, elution, and detection procedures were performed sequentially in the sequential injection lab-on-valve (SI-LOV) system followed by electrothermal atomic absorption spectrometry (ETAAS). Mixtures of hydrophobic analytes were successfully extracted from solution using the synthesized magnetic adsorbents. The potential use of the established scheme was demonstrated by taking cobalt as a model analyte. Under the optimal conditions, the calibration curve showed an excellent linearity in the concentration range of 0.01–5 μg L−1, and the relative standard deviation was 2.8% at the 0.5 μg L−1 level (n = 11). The limit of detection was 6 ng L−1 with a sampling frequency of 18 h−1. The present method has been successfully applied to cobalt determination in water samples and two certified reference materials.

  20. An automatic micro-sequential injection bead injection lab-on-valve (muSI-BI-LOV) assembly for speciation analysis of ultra trace levels of Cr(III) and Cr(VI) incorporating on-line chemical reduction and employing detection by electrothermal atomic absorption spectrometry (ETAAS)

    DEFF Research Database (Denmark)

    Long, Xiangbao; Miró, Manuel; Hansen, Elo Harald

    2005-01-01

    and determination of trace levels of Cr(III) and Cr(VI) in environmental samples. The method was validated by determination of chromium species in CRM and NIST standard reference materials, and by spike recoveries of surface waters. Statistical comparison of means between experimental results and the total chromium...... certified values for the CRM and NIST materials revealed the non-existence of significant differences at a 95% confidence level....

  1. Determination of trace zinc in seawater by coupling solid phase extraction and fluorescence detection in the Lab-On-Valve format.

    Science.gov (United States)

    Grand, Maxime M; Chocholouš, Petr; Růžička, Jarda; Solich, Petr; Measures, Christopher I

    2016-06-01

    By virtue of their compactness, long-term stability, minimal reagent consumption and robustness, miniaturized sequential injection instruments are well suited for automation of assays onboard research ships. However, in order to reach the sensitivity and limit of detection required for open-ocean determinations of trace elements, it is necessary to preconcentrate the analyte prior its derivatization and subsequent detection by fluorescence. In this work, a novel method for the determination of dissolved zinc (Zn) at subnanomolar levels in seawater is described. The proposed method combines, for the first time, automated matrix removal, extraction of the target element, and fluorescence detection within a miniaturized flow manifold, based on the Lab-On-Valve (LOV) concept. The key feature of the microfluidic manipulation of the sample is flow programming, designed to pass sample through a mini-column where the target analyte and other complexable cations are retained, while the seawater matrix is washed out. Next, zinc is eluted and merged with a Zn selective fluorescent probe (FluoZin-3) at the confluence point of the LOV central channel using two high-precision stepper motor driven pumps that are operated in concert. Finally, the thus formed Zn complex is transported to the LOV flow cell for selective fluorescence measurement. This work describes the characterization and optimization of the method including Solid Phase Extraction using the Toyopearl AF-Chelate-650M resin, and detailed assay protocol controlled by a commercially available software and instrument. The proposed method features a LOD of 0.02 nM, high precision (<3% at 0.1 and 2 nM Zn levels), an assay cycle of 13 min and a reagent consumption of 150 μL FluoZin-3 per sample, which makes the method highly suitable for oceanographic shipboard analysis. The accuracy of the method has been validated through the analysis of seawater reference standards and comparison with ICP-MS determinations on

  2. Multi-walled carbon nanotubes and metal-organic framework nanocomposites as novel hybrid electrode materials for the determination of nano-molar levels of lead in a lab-on-valve format.

    Science.gov (United States)

    Wang, Yang; Wu, Yichun; Xie, Jing; Ge, Huali; Hu, Xiaoya

    2013-09-01

    Metal-organic frameworks have been the subject of intense research because of their unique physicochemical properties. The presented study investigates the application of multi-wall carbon nanotubes and metal-organic frameworks (MWCNTs@Cu3(BTC)2) nanoparticles-modified electrode for the determination of trace levels of lead. The nanocomposites were prepared by solvothermal synthesis and characterized in detail. The experimental procedure was carried out by accumulating lead on the electrode surface and subsequently measuring with differential pulse anodic stripping voltammetry in a lab-on-valve format. The main parameters affecting the analytical performance, including the amount of MWCNTs@Cu3(BTC)2 suspension, supporting electrolyte and its pH, stripping mode, and flow rate, have been investigated in detail. Under the optimum conditions, the oxidation peak current displayed a calibration response for lead over a concentration range from 1.0 × 10(-9) to 5.0 × 10(-8) mol L(-1) with a excellent detection limit of 7.9 × 10(-10) mol L(-1). The relative standard deviation of 7 successive scans was 3.10% for 1.0 × 10(-8) mol L(-1) lead. The established method showed a great improvement in sensitivity and sample throughput for lead analysis. PMID:23853779

  3. Immanuel and Me With-Out Hyphen

    OpenAIRE

    Andre Gunder Frank

    2015-01-01

    This essay is my personal and intellectual tribute to Immanuel Wallerstein. It takes the form of my also personal intellectual account of our ?rst independent, then joint, and again increasingly separate journeys through the maze of the world [-] system with and without a hyphen. Imagine our relations as a horizontal Y shaped rope. It began with strands that, in the 1960s, ran parallel, becoming intertwined during the 1970s and 1980s until the strands (or at least some) separated again in the...

  4. Immanuel and Me With-Out Hyphen

    Directory of Open Access Journals (Sweden)

    Andre Gunder Frank

    2015-08-01

    Full Text Available This essay is my personal and intellectual tribute to Immanuel Wallerstein. It takes the form of my also personal intellectual account of our ?rst independent, then joint, and again increasingly separate journeys through the maze of the world [-] system with and without a hyphen. Imagine our relations as a horizontal Y shaped rope. It began with strands that, in the 1960s, ran parallel, becoming intertwined during the 1970s and 1980s until the strands (or at least some separated again in the 1990s, going off in increasingly different directions like a horizontal Y. Why? My answer is both circumstantial and personal, in which the personal choices and trajectories are driven primarily by world and local political circumstance. Of course, my account re?ects my own perspective on this story. However it also includes other colleagues and friends of Immanuel’s and mine, in particular our co-authors in several books and edited volumes, Giovanni Arrighi and Samir Amin, with whom I can check this account. Others, alas, are no longer with us.

  5. The Hyphen as a Syllabification Cue in Reading Bisyllabic and Multisyllabic Words among Finnish 1st and 2nd Graders

    Science.gov (United States)

    Häikiö, Tuomo; Bertram, Raymond; Hyönä, Jukka

    2016-01-01

    Finnish ABC books present words with hyphens inserted at syllable boundaries. Syllabification by hyphens is abandoned in the 2nd grade for bisyllabic words, but continues for words with three or more syllables. The current eye movement study investigated how and to what extent syllable hyphens in bisyllabic ("kah-vi" "cof-fee")…

  6. Polymer architectures via mass spectrometry and hyphenated techniques: A review.

    Science.gov (United States)

    Crotty, Sarah; Gerişlioğlu, Selim; Endres, Kevin J; Wesdemiotis, Chrys; Schubert, Ulrich S

    2016-08-17

    This review covers the application of mass spectrometry (MS) and its hyphenated techniques to synthetic polymers of varying architectural complexities. The synthetic polymers are discussed as according to their architectural complexity from linear homopolymers and copolymers to stars, dendrimers, cyclic copolymers and other polymers. MS and tandem MS (MS/MS) has been extensively used for the analysis of synthetic polymers. However, the increase in structural or architectural complexity can result in analytical challenges that MS or MS/MS cannot overcome alone. Hyphenation to MS with different chromatographic techniques (2D × LC, SEC, HPLC etc.), utilization of other ionization methods (APCI, DESI etc.) and various mass analyzers (FT-ICR, quadrupole, time-of-flight, ion trap etc.) are applied to overcome these challenges and achieve more detailed structural characterizations of complex polymeric systems. In addition, computational methods (software: MassChrom2D, COCONUT, 2D maps etc.) have also reached polymer science to facilitate and accelerate data interpretation. Developments in technology and the comprehension of different polymer classes with diverse architectures have significantly improved, which allow for smart polymer designs to be examined and advanced. We present specific examples covering diverse analytical aspects as well as forthcoming prospects in polymer science. PMID:27286765

  7. New Developments in LC-MS and Other Hyphenated Techniques

    Energy Technology Data Exchange (ETDEWEB)

    Belov, Mikhail E.; Kurulugama, Ruwan T.; Lopez-Ferrer, Daniel; Ibrahim, Yehia M.; Baker, Erin Shammel

    2011-06-21

    Extensive challenges faced by analytical chemists in studying real world complex samples such as biological body fluids, tissue samples, environmental and geological samples have lead to the development of advanced analytical approaches. The vast array of contemporary technologies can be categorized into two major areas: sample separation and mass spectrometry analysis. Current state-of-the-art sample separation methods include gas chromatography, high performance liquid chromatography, ultra high pressure liquid chromatography, solid phase extraction, capillary electrophoresis, and gas phase separation techniques such as ion mobility spectrometry. The recent trend in sample separation is to combine (or hyphenate) multiple techniques that employ different separation mechanisms to maximize separation efficiency. The most widely used combinations include two-dimensional gas chromatography, strong cation exchange or weak cation exchange chromatography followed by reversed-phase liquid chromatography, two-dimensional reversed-phase liquid chromatography, liquid chromatography followed by ion mobility spectrometry and two-dimensional electrophoresis techniques. The introduction of atmospheric pressure ionization techniques such as electrospray ionization and matrix assisted laser desorption ionization and variations of the two have drastically increased the impact of mass spectrometry on bioanalytical applications. Mass spectrometry itself has tremendously improved over the years in terms of sensitivity, detection limits, dynamic range and sequencing capabilities. Currently, mass spectrometers can attain zeptomolole detection limits with five orders of magnitude dynamic range. In this chapter, we summarize recent developments in hyphenated techniques and their applications to complex sample analysis.

  8. Editor's intervention in the register of compounds in archaic Portuguese texts: some reflections on the use of hyphen

    Directory of Open Access Journals (Sweden)

    Antonia Vieira dos Santos

    2014-07-01

    Full Text Available The use of hyphen within compounds was not built up before the nineteenth century. Thus, compounds spelled with hyphen in archaic Portuguese texts are a result of editing criteria adopted by editors. From this type of intervention, the relationship between hyphen use – result of a spelling convention – and the definition of compound adopted by the editor are discussed. Its absence is significant to the history of the language.

  9. The Three Generations of Flow Injection Analysis

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Wang, Jianhua

    2004-01-01

    The characteristics of the three generations of flow injection analysis, that is, FIA, sequential injection analysis (SIA), and bead injection-lab-on-valve (BI-LOV), are briefly outlined, their individual advantages and shortcomings are discussed, and selected practical applications are presented....

  10. New method for speciation analysis of aluminium fluoride complexes by HPLC-FAAS hyphenated technique.

    Science.gov (United States)

    Frankowski, M; Zioła-Frankowska, A; Siepak, J

    2010-03-15

    Speciation analysis of aluminium in the presented system of HPLC-FAAS hyphenated technique lasts 4min. Using the bifunctional column in model analysis and using the calculation methods for modelling using the Mineql program enabled the authors to presume that particular forms will be subjected to elution in the following order: (1) AlF(2)(+) and AlF(4)(-), (2) AlF(2+) and AlF(3)(0) and (3) Al(3+). Based on the obtained results for model solutions, the presented method enables the determination of aluminium fluoride complexes and Al(3+) speciation form. The study compares the tendency of occurrence variability of aluminium fluoride complexes and Al(3+) form, determined based on the results obtained using the HPLC-FAAS hyphenated technique with the trend defined based on the Mineql program calculation method. The method was successfully applied to soil samples. PMID:20152461

  11. Identification and characterization of related substances in pomalidomide by hyphenated LC-MS techniques.

    Science.gov (United States)

    Lu, Ping; Wang, Lei; Song, Min; Hang, Tai-Jun

    2015-10-10

    The current study dealt with the separation, identification and characterization of related substances in pomalidomide by hyphenated techniques. Complete separation was obtained with an Inertsil ODS-SP column (250 mm × 4.6 mm, 5 μm) by linear gradient elution using a mobile phase consisting of 0.1% formic acid solution and acetonitrile. They were characterized by hyphenated chromatographic techniques with the accurate mass determination using high resolution LC-TOF-MS methods as well as the product MS spectra determination and elucidation. The degradation behaviors of pomalidomide under ICH prescribed stress conditions were also conducted. Pomalidomide was found to be labile to degrade under acid, alkaline, oxidative and thermal stress conditions, while it was relatively stable to photolytic stress. 13 related substances were detected and identified to be 10 degradation products and three process related substances. The hyphenated LC-MS method with high resolution accurate mass determination facilitated the qualitative analysis of the unknown compounds than that of the conventional HPLC-UV. The related compounds identified are valuable for pomalidomide manufacturing process optimization and quality control.

  12. Application of Hyphenated Techniques in Speciation Analysis of Arsenic, Antimony, and Thallium

    Directory of Open Access Journals (Sweden)

    Rajmund Michalski

    2012-01-01

    Full Text Available Due to the fact that metals and metalloids have a strong impact on the environment, the methods of their determination and speciation have received special attention in recent years. Arsenic, antimony, and thallium are important examples of such toxic elements. Their speciation is especially important in the environmental and biomedical fields because of their toxicity, bioavailability, and reactivity. Recently, speciation analytics has been playing a unique role in the studies of biogeochemical cycles of chemical compounds, determination of toxicity and ecotoxicity of selected elements, quality control of food products, control of medicines and pharmaceutical products, technological process control, research on the impact of technological installation on the environment, examination of occupational exposure, and clinical analysis. Conventional methods are usually labor intensive, time consuming, and susceptible to interferences. The hyphenated techniques, in which separation method is coupled with multidimensional detectors, have become useful alternatives. The main advantages of those techniques consist in extremely low detection and quantification limits, insignificant interference, influence as well as high precision and repeatability of the determinations. In view of their importance, the present work overviews and discusses different hyphenated techniques used for arsenic, antimony, and thallium species analysis, in different clinical, environmental and food matrices.

  13. MetAlign: Interface-Driven, Versatile Metabolomics Tool for Hyphenated Full-Scan Mass Spectrometry Data Preprocessing

    NARCIS (Netherlands)

    Lommen, A.

    2009-01-01

    Hyphenated full-scan MS technology creates large amounts of data. A versatile easy to handle automation tool aiding in the data analysis is very important in handling such a data stream. MetAlign software-as described in this manuscript-handles a broad range of accurate mass and nominal mass GC/MS a

  14. HPTLC Hyphenated with FTIR: Principles, Instrumentation and Qualitative Analysis and Quantitation

    Science.gov (United States)

    Cimpoiu, Claudia

    In recent years, much effort has been devoted to the coupling of high-performance thin-layer chromatography (HPTLC) with spectrometric methods because of the robustness and simplicity of HPTLC and the need for detection techniques that provide identification and determination of sample constituents. IR is one of the spectroscopic methods that have been coupled with HPTLC. IR spectroscopy has a high potential for the elucidation of molecular structures, and the characteristic absorption bands can be used for compound-specific detection. HPTLC-FTIR coupled method has been widely used in the modern laboratories for the qualitative and quantitative analysis. The potential of this method is demonstrated by its application in different fields of analysis such as drug analysis, forensic analysis, food analysis, environmental analysis, biological analysis, etc. The hyphenated HPTLC-FTIR technique will be developed in the future with the aim of taking full advantage of this method.

  15. Real-time 2D separation by LC × differential ion mobility hyphenated to mass spectrometry.

    Science.gov (United States)

    Varesio, Emmanuel; Le Blanc, J C Yves; Hopfgartner, Gérard

    2012-03-01

    The liquid chromatography-mass spectrometry (LC-MS) analysis of complex samples such as biological fluid extracts is widespread when searching for new biomarkers as in metabolomics. The success of this hyphenation resides in the orthogonality of both separation techniques. However, there are frequent cases where compounds are co-eluting and the resolving power of mass spectrometry (MS) is not sufficient (e.g., isobaric compounds and interfering isotopic clusters). Different strategies are discussed to solve these cases and a mixture of eight compounds (i.e., bromazepam, chlorprothixene, clonapzepam, fendiline, flusilazol, oxfendazole, oxycodone, and pamaquine) with identical nominal mass (i.e., m/z 316) is taken to illustrate them. Among the different approaches, high-resolution mass spectrometry or liquid chromatography (i.e., UHPLC) can easily separate these compounds. Another technique, mostly used with low resolving power MS analyzers, is differential ion mobility spectrometry (DMS), where analytes are gas-phase separated according to their size-to-charge ratio. Detailed investigations of the addition of different polar modifiers (i.e., methanol, ethanol, and isopropanol) into the transport gas (nitrogen) to enhance the peak capacity of the technique were carried out. Finally, a complex urine sample fortified with 36 compounds of various chemical properties was analyzed by real-time 2D separation LC×DMS-MS(/MS). The addition of this orthogonal gas-phase separation technique in the LC-MS(/MS) hyphenation greatly improved data quality by resolving composite MS/MS spectra, which is mandatory in metabolomics when performing database generation and search. PMID:22006241

  16. SFC-APLI-(TOF)MS: Hyphenation of Supercritical Fluid Chromatography to Atmospheric Pressure Laser Ionization Mass Spectrometry.

    Science.gov (United States)

    Klink, Dennis; Schmitz, Oliver Johannes

    2016-01-01

    Atmospheric-pressure laser ionization mass spectrometry (APLI-MS) is a powerful method for the analysis of polycyclic aromatic hydrocarbon (PAH) molecules, which are ionized in a selective and highly sensitive way via resonance-enhanced multiphoton ionization. APLI was presented in 2005 and has been hyphenated successfully to chromatographic separation techniques like high performance liquid chromatography (HPLC) and gas chromatography (GC). In order to expand the portfolio of chromatographic couplings to APLI, a new hyphenation setup of APLI and supercritical-fluid chromatography (SFC) was constructed and aim of this work. Here, we demonstrate the first hyphenation of SFC and APLI in a simple designed way with respect to different optimization steps to ensure a sensitive analysis. The new setup permits qualitative and quantitative determination of native and also more polar PAH molecules. As a result of the altered ambient characteristics within the source enclosure, the quantification of 1-hydroxypyrene (1-HP) in human urine is possible without prior derivatization. The limit of detection for 1-HP by SFC-APLI-TOF(MS) was found to be 0.5 μg L(-1), which is lower than the 1-HP concentrations found in exposed persons. PMID:26633261

  17. Screening of cadmium and lead in potentially contaminated waters using a spectrophotometric sequential injection lab-on-valve methodology.

    Science.gov (United States)

    Santos, Inês C; Mesquita, Raquel B R; Rangel, António O S S

    2015-10-01

    The present work describes the development of a µSI-LOV method for the simultaneous screening of cadmium and lead in potentially contaminated water samples. To attain the biparametric determination, dithizone was chosen as the spectrophotometric reagent as it forms a colored complex with both metal ions, at different pH conditions. The cadmium determination was attained in strong alkaline conditions (pH≈12); the lead determination was calculated by the difference with the determination of both metals in mild alkaline conditions (pH≈8). The colored complex was measured at 550 nm and the method presented a LOD of 34 μg L(-1) for cadmium and 56 μg L(-1) for lead, with a sample consumption of 20 µL per assay and a determination rate of 55 h(-1). The results obtained were in agreement with those obtained by FAAS. The developed method was efficiently applied to the screening of cadmium and lead in marine port waters. PMID:26078171

  18. Chromatographic analysis of Polygalae Radix by online hyphenating pressurized liquid extraction

    Science.gov (United States)

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

    2016-01-01

    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. PMID:27272557

  19. Chromatographic analysis of Polygalae Radix by online hyphenating pressurized liquid extraction

    Science.gov (United States)

    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.

  20. Hyphenated GC-FTIR and GC-MS techniques applied in the analysis of bioactive compounds

    Science.gov (United States)

    Gosav, Steluta; Paduraru, Nicoleta; Praisler, Mirela

    2014-08-01

    The drugs of abuse, which affect human nature and cause numerous crimes, have become a serious problem throughout the world. There are hundreds of amphetamine analogues on the black market. They consist of various alterations of the basic amphetamine molecular structure, which are yet not yet included in the lists of forbidden compounds although they retain or slightly modify the hallucinogenic effects of their parent compound. It is their important variety that makes their identification quite a challenge. A number of analytical procedures for the identification of amphetamines and their analogues have recently been reported. We are presenting the profile of the main hallucinogenic amphetamines obtained with the hyphenated techniques that are recommended for the identification of illicit amphetamines, i. e. gas chromatography combined with mass spectrometry (GC-MS) and gas chromatography coupled with Fourier transform infrared spectrometry (GC-FTIR). The infrared spectra of the analyzed hallucinogenic amphetamines present some absorption bands (1490 cm-1, 1440 cm-1, 1245 cm-1, 1050 cm-1 and 940 cm-1) that are very stable as position and shape, while their intensity depends of the side-chain substitution. The specific ionic fragment of the studied hallucinogenic compounds is the 3,4-methylenedioxybenzyl cation (m/e = 135) which has a small relative abundance (lesser than 20%). The complementarity of the above mentioned techniques for the identification of hallucinogenic compounds is discussed.

  1. Chemometric profile of root extracts of Rhodiola imbricata Edgew. with hyphenated gas chromatography mass spectrometric technique.

    Science.gov (United States)

    Tayade, Amol B; Dhar, Priyanka; Kumar, Jatinder; Sharma, Manu; Chauhan, Rajinder S; Chaurasia, Om P; Srivastava, Ravi B

    2013-01-01

    Rhodiola imbricata Edgew. (Rose root or Arctic root or Golden root or Shrolo), belonging to the family Crassulaceae, is an important food crop and medicinal plant in the Indian trans-Himalayan cold desert. Chemometric profile of the n-hexane, chloroform, dichloroethane, ethyl acetate, methanol, and 60% ethanol root extracts of R. imbricata were performed by hyphenated gas chromatography mass spectrometry (GC/MS) technique. GC/MS analysis was carried out using Thermo Finnigan PolarisQ Ion Trap GC/MS MS system comprising of an AS2000 liquid autosampler. Interpretation on mass spectrum of GC/MS was done using the NIST/EPA/NIH Mass Spectral Database, with NIST MS search program v.2.0g. Chemometric profile of root extracts revealed the presence of 63 phyto-chemotypes, among them, 1-pentacosanol; stigmast-5-en-3-ol, (3β,24S); 1-teracosanol; 1-henteracontanol; 17-pentatriacontene; 13-tetradecen-1-ol acetate; methyl tri-butyl ammonium chloride; bis(2-ethylhexyl) phthalate; 7,8-dimethylbenzocyclooctene; ethyl linoleate; 3-methoxy-5-methylphenol; hexadecanoic acid; camphor; 1,3-dimethoxybenzene; thujone; 1,3-benzenediol, 5-pentadecyl; benzenemethanol, 3-hydroxy, 5-methoxy; cholest-4-ene-3,6-dione; dodecanoic acid, 3-hydroxy; octadecane, 1-chloro; ethanone, 1-(4-hydroxyphenyl); α-tocopherol; ascaridole; campesterol; 1-dotriacontane; heptadecane, 9-hexyl were found to be present in major amount. Eventually, in the present study we have found phytosterols, terpenoids, fatty acids, fatty acid esters, alkyl halides, phenols, alcohols, ethers, alkanes, and alkenes as the major group of phyto-chemotypes in the different root extracts of R. imbricata. All these compounds identified by GC/MS analysis were further investigated for their biological activities and it was found that they possess a diverse range of positive pharmacological actions. In future, isolation of individual phyto-chemotypes and subjecting them to biological activity will definitely prove fruitful results in

  2. Chemometric profile of root extracts of Rhodiola imbricata Edgew. with hyphenated gas chromatography mass spectrometric technique.

    Directory of Open Access Journals (Sweden)

    Amol B Tayade

    Full Text Available Rhodiola imbricata Edgew. (Rose root or Arctic root or Golden root or Shrolo, belonging to the family Crassulaceae, is an important food crop and medicinal plant in the Indian trans-Himalayan cold desert. Chemometric profile of the n-hexane, chloroform, dichloroethane, ethyl acetate, methanol, and 60% ethanol root extracts of R. imbricata were performed by hyphenated gas chromatography mass spectrometry (GC/MS technique. GC/MS analysis was carried out using Thermo Finnigan PolarisQ Ion Trap GC/MS MS system comprising of an AS2000 liquid autosampler. Interpretation on mass spectrum of GC/MS was done using the NIST/EPA/NIH Mass Spectral Database, with NIST MS search program v.2.0g. Chemometric profile of root extracts revealed the presence of 63 phyto-chemotypes, among them, 1-pentacosanol; stigmast-5-en-3-ol, (3β,24S; 1-teracosanol; 1-henteracontanol; 17-pentatriacontene; 13-tetradecen-1-ol acetate; methyl tri-butyl ammonium chloride; bis(2-ethylhexyl phthalate; 7,8-dimethylbenzocyclooctene; ethyl linoleate; 3-methoxy-5-methylphenol; hexadecanoic acid; camphor; 1,3-dimethoxybenzene; thujone; 1,3-benzenediol, 5-pentadecyl; benzenemethanol, 3-hydroxy, 5-methoxy; cholest-4-ene-3,6-dione; dodecanoic acid, 3-hydroxy; octadecane, 1-chloro; ethanone, 1-(4-hydroxyphenyl; α-tocopherol; ascaridole; campesterol; 1-dotriacontane; heptadecane, 9-hexyl were found to be present in major amount. Eventually, in the present study we have found phytosterols, terpenoids, fatty acids, fatty acid esters, alkyl halides, phenols, alcohols, ethers, alkanes, and alkenes as the major group of phyto-chemotypes in the different root extracts of R. imbricata. All these compounds identified by GC/MS analysis were further investigated for their biological activities and it was found that they possess a diverse range of positive pharmacological actions. In future, isolation of individual phyto-chemotypes and subjecting them to biological activity will definitely prove fruitful

  3. Instrumentation of High Temperature and Pressure Reaction System with Continuous Flow and Its Hyphenation to a Liquid Chromatograph

    OpenAIRE

    Tsuda, Takao; Kitagawa, Shinya; Umeyama, Takayuki; Araki, Shuki; Hirashita, Tsunehisa; Aoki, Mutsumi; Nakamura, Koichi; キタガワ, シンヤ; アラキ, シュウキ; ヒラシタ, ツネヒサ; アオキ, ムツミ; 北川, 慎也; 荒木, 修喜; 平下, 恒久; 青木, 睦

    2006-01-01

    A continuous flow-type hydrothermal reaction system, in which both temperature and pressure were rapidly and dynamically controlled, was constructed. It is called a real time high temperature and pressure reaction system (RT-HighTP). The RT-HighTP was hyphenated with liquid chromatograph (RT-HighTP-LC) to achieve prompt analysis of the reaction products. The RT-HighTP system produced stable pressure under the supercritical and subcritical phases (%RSD < 3%). The RT-HighTP-LC was able to chang...

  4. Determination of Oleanolic and Ursolic Acids in Hedyotis diffusa Using Hyphenated Ultrasound-Assisted Supercritical Carbon Dioxide Extraction and Chromatography

    OpenAIRE

    Ming-Chi Wei; Yu-Chiao Yang; Show-Jen Hong

    2015-01-01

    Oleanolic acid (OA) and ursolic acid (UA) were extracted from Hedyotis diffusa using a hyphenated procedure of ultrasound-assisted and supercritical carbon dioxide (HSC–CO2) extraction at different temperatures, pressures, cosolvent percentages, and SC–CO2 flow rates. The results indicated that these parameters significantly affected the extraction yield. The maximal yields of OA (0.917 mg/g of dry plant) and UA (3.540 mg/g of dry plant) were obtained at a dynamic extraction time of 110 min, ...

  5. 英语构词法中连字符构词功能分析%The Compounding Function of Hyphen in English Word-Building

    Institute of Scientific and Technical Information of China (English)

    李凤东

    2010-01-01

    连字符(hyphen)是英语书面语中一个常见符号,除一些基本语法功能外,连字符(hyphen)还具有很强的构词功能,这在很大程度上弥补了派生、转性等构词法的不足,在英语学习过程中我们应对连字符的构词功能给予足够重视.

  6. Hyphenation of sequential- and flow injection analysis with FTIR-spectroscopy for chemical analysis in aqueous solutions

    Science.gov (United States)

    Lendl, B.; Schindler, R.; Kellner, R.

    1998-06-01

    A survey of the principles of sequential (SIA)-and flow injection analysis (FIA) systems with FTIR spectroscopic detection is presented to introduce these hyphenations as powerful techniques for performing chemical analysis in aqueous solution. The strength of FIA/SIA-FTIR systems lies in the possibility to perform highly reproducible and automated sample manipulations such as sample clean-up and/or chemical reactions prior to spectrum acquisition. It is shown that the hyphenation of FIA/SIA systems with an FTIR spectrometer enhances the problem solving capabilities of the FTIR spectrometer as also parameters which can not be measured directly (e.g. enzyme activities) can be determined. On the other hand application of FTIR spectroscopic detection in FIA or SIA is also of advantage as it allows to shorten conventional analysis procedures (e.g. sucrose or phosphate analysis) or to establish and apply a multivariate calibration model for simultaneous determinations (e.g. glucose, fructose and sucrose analysis). In addition to these examples two recent instrumental developments in miniaturized FIA/SIA-FTIR systems, a μ-Flow through cell based on IR fiber optics and a micromachined SI-enzyme reactor are presented in this paper.

  7. Determination of Oleanolic and Ursolic Acids in Hedyotis diffusa Using Hyphenated Ultrasound-Assisted Supercritical Carbon Dioxide Extraction and Chromatography

    Directory of Open Access Journals (Sweden)

    Ming-Chi Wei

    2015-01-01

    Full Text Available Oleanolic acid (OA and ursolic acid (UA were extracted from Hedyotis diffusa using a hyphenated procedure of ultrasound-assisted and supercritical carbon dioxide (HSC–CO2 extraction at different temperatures, pressures, cosolvent percentages, and SC–CO2 flow rates. The results indicated that these parameters significantly affected the extraction yield. The maximal yields of OA (0.917 mg/g of dry plant and UA (3.540 mg/g of dry plant were obtained at a dynamic extraction time of 110 min, a static extraction time of 15 min, 28.2 MPa, and 56°C with a 12.5% (v/v cosolvent (ethanol/water = 82/18, v/v and SC–CO2 flowing at 2.3 mL/min (STP. The extracted yields were then analyzed by high performance liquid chromatography (HPLC to quantify the OA and UA. The present findings revealed that H. diffusa is a potential source of OA and UA. In addition, using the hyphenated procedure for extraction is a promising and alternative process for recovering OA and UA from H. diffusa at high concentrations.

  8. Determination of Oleanolic and Ursolic Acids in Hedyotis diffusa Using Hyphenated Ultrasound-Assisted Supercritical Carbon Dioxide Extraction and Chromatography.

    Science.gov (United States)

    Wei, Ming-Chi; Yang, Yu-Chiao; Hong, Show-Jen

    2015-01-01

    Oleanolic acid (OA) and ursolic acid (UA) were extracted from Hedyotis diffusa using a hyphenated procedure of ultrasound-assisted and supercritical carbon dioxide (HSC-CO2) extraction at different temperatures, pressures, cosolvent percentages, and SC-CO2 flow rates. The results indicated that these parameters significantly affected the extraction yield. The maximal yields of OA (0.917 mg/g of dry plant) and UA (3.540 mg/g of dry plant) were obtained at a dynamic extraction time of 110 min, a static extraction time of 15 min, 28.2 MPa, and 56°C with a 12.5% (v/v) cosolvent (ethanol/water = 82/18, v/v) and SC-CO2 flowing at 2.3 mL/min (STP). The extracted yields were then analyzed by high performance liquid chromatography (HPLC) to quantify the OA and UA. The present findings revealed that H. diffusa is a potential source of OA and UA. In addition, using the hyphenated procedure for extraction is a promising and alternative process for recovering OA and UA from H. diffusa at high concentrations. PMID:26089939

  9. Hyphenation of infrared spectroscopy to liquid chromatography for qualitative and quantitative polymer analysis: Degradation of poly(bisphenol A)carbonate

    NARCIS (Netherlands)

    Coulier, L.; Kaal, E.; Hankemeier, T.

    2006-01-01

    Hyphenation of infrared spectroscopy (IR) to liquid chromatography (LC) has been applied to study chemical changes in poly(bisphenol A)carbonate (PC) as a result of degradation. Especially coupling of LC to FTIR through solvent elimination is a sensitive approach to identify changes in functionality

  10. Hyphenation of aqueous liquid chromatography to pyrolysis-gas chromatography and mass spectrometry for the comprehensive characterization of water-soluble polymers

    NARCIS (Netherlands)

    E.R. Kaal; M. Kurano; M. Geissler; H.-G. Janssen

    2008-01-01

    A recently developed hyphenated system for "organic" size-exclusion chromatography-pyrolysis-gas chromatography-mass spectrometry (SEC-Py-GC-MS) is adapted to allow the use of aqueous LC eluents as applied in the characterization of water-soluble polymers. The system uses syringe-based transfer of m

  11. Two-dimensional separation of ionic species by hyphenation of capillary ion chromatography × capillary electrophoresis-mass spectrometry.

    Science.gov (United States)

    Beutner, Andrea; Kochmann, Sven; Mark, Jonas Josef Peter; Matysik, Frank-Michael

    2015-03-17

    The separation of complex mixtures such as biological or environmental samples requires high peak capacities, which cannot be established with a single separation technique. Therefore, multidimensional systems are in demand. In this work, we present the hyphenation of the two most important (orthogonal) techniques in ion analysis, namely, ion chromatography (IC) and capillary electrophoresis (CE), in combination with mass spectrometry. A modulator was developed ensuring a well-controlled coupling of IC and CE separations. Proof-of-concept measurements were performed using a model system consisting of nucleotides and cyclic nucleotides. The data are presented in a multidimensional contour plot. Analyte stacking in the CE separation could be exploited on the basis of the fact that the suppressed IC effluent is pure water.

  12. Hyphenation of two simultaneously employed soft photo ionization mass spectrometers with thermal analysis of biomass and biochar

    International Nuclear Information System (INIS)

    Highlights: ► First simultaneous hyphenation of two time-of-flight mass spectrometers with different soft photo ionization techniques (SPI and REMPI) to Thermal Analysis using a newly developed prototype for EGA is presented. ► Resonance enhanced multi-photon ionization (REMPI) enables sensitive and selective analysis of aromatic species. ► Single photon ionization (SPI) using VUV light supplied by an innovative electron-beam pumped excimer light source (EBEL) comprehensively ionizes (nearly) all organic molecules. ► The resulting mass spectra show distinct patterns for the evolved gases of the miscellaneous biomasses and chars thereof. ► The potential for detailed kinetic studies is apparent on account of the complex pyrolysis gas compositions. - Abstract: Evolved gas analysis (EGA) is a powerful and complementary tool for Thermal Analysis. In this context, two time-of-flight mass spectrometers with different soft photo-ionization techniques are simultaneously hyphenated to a thermo balance and applied in form of a newly developed prototype for EGA of pyrolysis gases from biomass and biochar. Resonance enhanced multi-photon ionization (REMPI) is applied for selective analysis of aromatic species. Furthermore, single photon ionization (SPI) using VUV light supplied by an electron-beam pumped excimer light source (EBEL) was used to comprehensively ionize (nearly) all organic molecules. The soft ionization capability of photo-ionization techniques allows direct and on-line analysis of the evolved pyrolysis gases. Characteristic mass spectra with specific patterns could be obtained for the miscellaneous biomass feeds used. Temperature profiles of the biochars reveal a desorption step, followed by pyrolysis as observed for the biomasses. Furthermore, the potential for kinetic studies is apparent for this instrumental setup.

  13. Electrospray-Differential Mobility Hyphenated with Single Particle Inductively Coupled Plasma Mass Spectrometry for Characterization of Nanoparticles and Their Aggregates.

    Science.gov (United States)

    Tan, Jiaojie; Liu, Jingyu; Li, Mingdong; El Hadri, Hind; Hackley, Vincent A; Zachariah, Michael R

    2016-09-01

    The novel hyphenation of electrospray-differential mobility analysis with single particle inductively coupled plasma mass spectrometry (ES-DMA-spICPMS) was demonstrated with the capacity for real-time size, mass, and concentration measurement of nanoparticles (NPs) on a particle-to-particle basis. In this proof-of-concept study, the feasibility of this technique was validated through both concentration and mass calibration using NIST gold NP reference materials. A detection limit of 10(5) NPs mL(-1) was determined under current experimental conditions, which is about 4 orders of magnitude lower in comparison to that of a traditional ES-DMA setup using a condensation particle counter as detector. Furthermore, independent and simultaneous quantification of both size and mass of NPs provides information regarding NP aggregation states. Two demonstrative applications include gold NP mixtures with a broad size range (30-100 nm), and aggregated gold NPs with a primary size of 40 nm. Finally, this technique was shown to be potentially useful for real-world samples with high ionic background due to its ability to remove dissolved ions yielding a cleaner background. Overall, we demonstrate the capacity of this new hyphenated technique for (1) clearly resolving NP populations from a mixture containing a broad size range; (2) accurately measuring a linear relationship, which should inherently exist between mobility size and one-third power of ICPMS mass for spherical NPs; (3) quantifying the early stage propagation of NP aggregation with well-characterized oligomers; and (4) differentiating aggregated NPs and nonaggregated states based on the "apparent density" derived from both DMA size and spICPMS mass. PMID:27479448

  14. Electrospray-Differential Mobility Hyphenated with Single Particle Inductively Coupled Plasma Mass Spectrometry for Characterization of Nanoparticles and Their Aggregates.

    Science.gov (United States)

    Tan, Jiaojie; Liu, Jingyu; Li, Mingdong; El Hadri, Hind; Hackley, Vincent A; Zachariah, Michael R

    2016-09-01

    The novel hyphenation of electrospray-differential mobility analysis with single particle inductively coupled plasma mass spectrometry (ES-DMA-spICPMS) was demonstrated with the capacity for real-time size, mass, and concentration measurement of nanoparticles (NPs) on a particle-to-particle basis. In this proof-of-concept study, the feasibility of this technique was validated through both concentration and mass calibration using NIST gold NP reference materials. A detection limit of 10(5) NPs mL(-1) was determined under current experimental conditions, which is about 4 orders of magnitude lower in comparison to that of a traditional ES-DMA setup using a condensation particle counter as detector. Furthermore, independent and simultaneous quantification of both size and mass of NPs provides information regarding NP aggregation states. Two demonstrative applications include gold NP mixtures with a broad size range (30-100 nm), and aggregated gold NPs with a primary size of 40 nm. Finally, this technique was shown to be potentially useful for real-world samples with high ionic background due to its ability to remove dissolved ions yielding a cleaner background. Overall, we demonstrate the capacity of this new hyphenated technique for (1) clearly resolving NP populations from a mixture containing a broad size range; (2) accurately measuring a linear relationship, which should inherently exist between mobility size and one-third power of ICPMS mass for spherical NPs; (3) quantifying the early stage propagation of NP aggregation with well-characterized oligomers; and (4) differentiating aggregated NPs and nonaggregated states based on the "apparent density" derived from both DMA size and spICPMS mass.

  15. Hyphenation of supercritical fluid chromatography and two-dimensional gas chromatography-mass spectrometry for group type separations.

    Science.gov (United States)

    Potgieter, H; van der Westhuizen, R; Rohwer, E; Malan, D

    2013-06-14

    The Fischer-Tropsch (FT) process produces a variety of compounds over a wide carbon number range and the synthetic crude oil produced by this process is rich in highly valuable olefins and oxygenates, which crude oil only contains at trace levels. The characterization of these products is very challenging even when using comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC×GC-TOF-MS). The separation between cyclic paraffins and olefins is especially difficult since they elute in similar positions on the GC×GC chromatogram and since they have identical molecular masses with indistinguishable fragmentation patterns. Previously, a high performance liquid chromatography (HPLC) fractionation procedure was used prior to GC×GC-TOF-MS analysis to distinguish between alkenes and alkanes, both cyclic and non-cyclic, however, there was co-elution of the solvents used in the HPLC fractionation procedure, and the volatile components in the gasoline sample and the dilution introduced by the off-line fractionation procedure made it very difficult to investigate components present at very low concentrations. The hyphenation of supercritical fluid chromatography (SFC) to GC×GC is less complicated and the removal of the supercritical CO2 can be easily achieved without any loss of the volatile sample components, eliminating the introduction of co-eluting solvents as well as the dilution effect. This paper describes the on-line hyphenation of SFC to a GC×GC system in order to comprehensively characterize the chemical groups (saturates, unsaturates, oxygenates and aromatics) in an FT sample. PMID:23647609

  16. The impact of flow injection on modem chemical analysis: has it fulfilled our expectations? And where are we going?

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    2004-01-01

    Presenting a condensation of the opening lecture of the 12th ICFIA conference, this communication presents a view of the impact that flow injection analysis (FIA) has had on modern analytical chemistry, evaluated both within the academic community and outside it, i.e., in “industry”. The ensuing...... developments of FIA, encompassing sequential injection analysis (SIA) and bead injection lab-on-valve (BI-LOV), are described and their individual features discussed. Finally some recent results of the activities from the author’s own research group are briefly mentioned....

  17. Surface enhanced Raman spectroscopy hyphenated with surface microextraction for in-situ detection of polycyclic aromatic hydrocarbons on food contact materials.

    Science.gov (United States)

    Zhang, Min; Zhang, Xiaoli; Shi, Yu-E; Liu, Zhen; Zhan, Jinhua

    2016-09-01

    Highly bioaccumulated polycyclic aromatic hydrocarbons (PAHs) have cause health concerns because of their carcinogenic properties. PAHs could migrate to food from contaminated food contact materials. In this study, a hyphenated technique combining surface enhanced Raman spectroscopy (SERS) with surface microextraction was developed for in-situ on site screening of PAHs on food contact materials. Methanol and 1-propanethiol-modified silver nanoparticles (PTH-Ag NPs) were used to perform the in-situ microextraction and detection of PAHs, respectively. The SERS spectra can be obtained by a portable Raman spectrometer. The vibration of the C-C bond of PTH at 1030cm(-1) was chosen as an internal standard peak. The PTH-Ag NPs showed high uniformity with an RSD of 2.96%. A plot of the normalized SERS intensity against fluoranthene concentration showed a linear relationship (R(2)=0.98). The detection limit could reach 0.27ngcm(-2). The in-situ microextraction-SERS hyphenated technique for the detection of three PAHs at five food contact materials was demonstrated. The method can be also applied to detect PAH mixtures. This in-situ microextraction-SERS hyphenated method demonstrated its ability to rapidly screen PAHs on contaminated food contact materials free from complex sample pretreatment. PMID:27343612

  18. A Hyphenated Technique based on High-Performance Thin Layer Chromatography for Determining Neutral Sphingolipids: A Proof of Concept

    Directory of Open Access Journals (Sweden)

    Andrés Domínguez

    2015-04-01

    Full Text Available Hyphenated HPTLC has been used to analyze several neutral sphingolipids acting as lysosomal storage disease (LSD biomarkers. Automated multiple development (AMD provides separation of lipid peaks, which are detected and quantified using fluorescence detection by intensity changes (FDIC after primuline post-impregnation. A final online transfer to a mass spectrometer by means of an elution-based interface allows their identification using electrospray ionization (ESI and atmospheric pressure chemical ionization (APCI.Given that the increases in fluorescent emission detected by FDIC are produced by non-specific, electrostatic interactions between the primuline and hydrocarbon chains in the ceramide backbones of sphingolipids, it is a non-destructive detection technique, allowing the precise location and transfer of biomarker peaks to a mass spectrometer using an elution interface. By using primuline as a fluorophore, the technique is also compatible with ESI-APCI and does not interfere with the MS of sphingolipids. APCI provides useful and complementary structural information to the ESI for sphingolipid identification. Moreover, FDIC emission can be used for quantitative purposes. Results include the determination of sphingomyelin (SM in human-plasma samples (RSD < 6% by means of a standard addition method with non-linear calibration, and the identification of globotriaosylceramide (Gb3 in the plasma of a Fabry patient. Only one HPTLC plate is needed to perform the analysis.

  19. Different Ways to On-Line Hyphenate Centrifugal Partition Chromatography and Mass Spectrometry: Application to Prenylated Xanthones from Garcinia mangostana.

    Science.gov (United States)

    Destandau, Emilie; Michel, Thomas; Toribio, Alix; Elfakir, Claire

    2015-11-01

    Centrifugal partition chromatography is a liquid-liquid separation method well adapted for the fractionation or purification of natural compounds from plant extracts. However, following the preparative isolation, the fractions collected must be analysed by high-performance thin-layer chromatography or high-performance liquid chromatography to evaluate their composition and/or their purity. These additional steps are time-consuming and increase the risk of compound degradation. In order to get an instantaneous analysis of fraction content with structural information on the phytochemicals eluted, it is possible to hyphenate on-line centrifugal partition chromatography with mass spectrometry. Depending on the complexity of the extract, two different kinds of centrifugal partition chromatography-mass spectrometry coupling can be performed: centrifugal partition chromatography-mass spectrometry or centrifugal partition chromatography-high-performance liquid chromatography-mass spectrometry coupling. In the first case, one part of the centrifugal partition chromatography effluent is directly introduced in the mass spectrometry ionisation source to identify the eluted compounds, while in the second case, it is directed to a high-performance liquid chromatography-mass spectrometry system where compounds are first separated thanks to high-performance liquid chromatography and then identified using mass spectrometry.

  20. High performance liquid chromatography hyphenated to inductively coupled plasma mass spectrometry for V and Ni quantification as tetrapyrroles

    Science.gov (United States)

    Duyck, Christiane Béatrice; Saint'Pierre, Tatiana Dillenburg; Miekeley, Norbert; da Fonseca, Teresa Cristina Oliveira; Szatmari, Peter

    2011-05-01

    A method was developed for the determination of V and Ni as tetrapyrroles by High Performance Liquid Chromatography hyphenated to Inductively Coupled Plasma Mass Spectrometry (HPLC-ICP-MS) using reversed phase and elution gradient. Chlorinated solvents and tetrahydrofuran were investigated as regard to separation time and ICP-MS detection efficiencies. The final elution gradient program started from pure methanol to a mixture of 20:80 (v/v) chloroform:methanol. External quantification of V and Ni with inorganic standards by flow injection ICP-MS, used online with HPLC, resulted in 95% of recoveries. The Limits of Detection for V during methanol elution and for Ni during the 20% chloroform gradient elution were evaluated by their minimum detectable concentrations, which were, respectively, 5 μg L - 1 and 8 μg L - 1 . The methodology was applied to polar and resin fractions separated from a Brazilian crude oil and a sediment extract from an oil-polluted area in the Guanabara Bay, Rio de Janeiro, Brazil. Vanadium as tetrapyrroles represented the totality of V content in the polar fraction, whereas Ni was in different polar forms in the resin and sediment extract.

  1. Different Ways to On-Line Hyphenate Centrifugal Partition Chromatography and Mass Spectrometry: Application to Prenylated Xanthones from Garcinia mangostana.

    Science.gov (United States)

    Destandau, Emilie; Michel, Thomas; Toribio, Alix; Elfakir, Claire

    2015-11-01

    Centrifugal partition chromatography is a liquid-liquid separation method well adapted for the fractionation or purification of natural compounds from plant extracts. However, following the preparative isolation, the fractions collected must be analysed by high-performance thin-layer chromatography or high-performance liquid chromatography to evaluate their composition and/or their purity. These additional steps are time-consuming and increase the risk of compound degradation. In order to get an instantaneous analysis of fraction content with structural information on the phytochemicals eluted, it is possible to hyphenate on-line centrifugal partition chromatography with mass spectrometry. Depending on the complexity of the extract, two different kinds of centrifugal partition chromatography-mass spectrometry coupling can be performed: centrifugal partition chromatography-mass spectrometry or centrifugal partition chromatography-high-performance liquid chromatography-mass spectrometry coupling. In the first case, one part of the centrifugal partition chromatography effluent is directly introduced in the mass spectrometry ionisation source to identify the eluted compounds, while in the second case, it is directed to a high-performance liquid chromatography-mass spectrometry system where compounds are first separated thanks to high-performance liquid chromatography and then identified using mass spectrometry. PMID:25615274

  2. Hyphenation of a Deoxyribonuclease I immobilized enzyme reactor with liquid chromatography for the online stability evaluation of oligonucleotides.

    Science.gov (United States)

    Álvarez Porebski, Piotr Wiktor; Gyssels, Ellen; Madder, Annemieke; Lynen, Frederic

    2015-11-27

    The stability of antisense oligonucleotides (ONs) toward nucleases is a key aspect for their possible implementation as therapeutic agents. Typically, ON stability studies are performed off-line, where the ONs are incubated with nucleases in solution, followed by their analysis. The problematics of off-line processing render the detailed comparison of relative ON stability quite challenging. Therefore, the development of an online platform based on an immobilized enzyme reactor (IMER) coupled to liquid chromatography (LC) was developed as an alternative for improved ON stability testing. More in detail, Deoxyribonuclease I (DNase I) was immobilized on epoxy-silica particles of different pore sizes and packed into a column for the construction of an IMER. Subsequently, the hyphenation of the IMER with ion-pair chromatography (IPC) and ion-exchange chromatography (IEC) was evaluated, leading to the successful development of two online methodologies: IMER-IPC and IMER-IEC. More specifically, natural and modified DNA and RNA oligonucleotides were used for testing the performance of the methodologies. Both methodologies proved to be simple, automatable, fast and highly reproducible for the quantitative and qualitative evaluation of ON degradation. In addition, the extended IMER life time in combination with a more straightforward control of the reaction kinetics substantiate the applicability of the IMER-LC platform for ON stability tests and its implementation in routine and research laboratories.

  3. Hyphenated and comprehensive liquid chromatography × gas chromatography-mass spectrometry for the identification of Mycobacterium tuberculosis.

    Science.gov (United States)

    Mourão, Marta P B; Denekamp, Ilse; Kuijper, Sjoukje; Kolk, Arend H J; Janssen, Hans-Gerd

    2016-03-25

    Tuberculosis is one of the world's most emerging public health problems, particularly in developing countries. Chromatography based methods have been used to tackle this epidemic by focusing on biomarker detection. Unfortunately, interferences from lipids in the sputum matrix, particularly cholesterol, adversely affect the identification and detection of the marker compounds. The present contribution describes the serial combination of normal phase liquid chromatography (NPLC) with thermally assisted hydrolysis and methylation followed by gas chromatography-mass spectrometry (THM-GC-MS) to overcome the difficulties of biomarker evaluation. The in-series combination consists of an LC analysis where fractions are collected and then transferred to the THM-GC-MS system. This was either done with comprehensive coupling, transferring all the fractions, or with hyphenated interfacing, i.e. off-line multi heart-cutting, transferring only selected fractions. Owing to the high sensitivity and selectivity of LC as a sample pre-treatment method, and to the high specificity of the MS as a detector, this analytical approach, NPLC × THM-GC-MS, is extremely sensitive. The results obtained indicate that this analytical set-up is able to detect down to 1 × 10(3) mycobacteria/mL of Mycobacterium tuberculosis strain 124, spiked in blank sputum samples. It is a powerful analytical tool and also has great potential for full automation. If further studies demonstrate its usefulness when applied blind in real sputum specimens, this technique could compete with the current smear microscopy in the early diagnosis of tuberculosis. PMID:26585206

  4. Characterization of the Axial Jet Separator with a CO2/Helium Mixture: Toward GC-AMS Hyphenation.

    Science.gov (United States)

    Salazar, G; Agrios, K; Eichler, R; Szidat, S

    2016-02-01

    Development of interfaces for sample introduction from high pressures is important for real-time online hyphenation of chromatographic and other separation devices with mass spectrometry (MS) or accelerator mass spectrometry (AMS). Momentum separators can reduce unwanted low-density gases and introduce the analyte into the vacuum. In this work, the axial jet separator, a new momentum interface, is characterized by theory and empirical optimization. The mathematical model describes the different axial penetration of the components of a jet-gas mixture and explains the empirical results for injections of CO2 in helium into MS and AMS instruments. We show that the performance of the new interface is sensitive to the nozzle size, showing good qualitative agreement with the mathematical model. Smaller nozzle sizes are more preferable due to their higher inflow capacity. The CO2 transmission efficiency of the interface into a MS instrument is ∼ 14% (CO2/helium separation factor of 2.7). The interface receives and delivers flows of ∼ 17.5 mL/min and ∼ 0.9 mL/min, respectively. For the interfaced AMS instrument, the ionization and overall efficiencies are 0.7-3% and 0.1-0.4%, respectively, for CO2 amounts of 4-0.6 μg C, which is only slightly lower compared to conventional systems using intermediate trapping. The ionization efficiency depends on to the carbon mass flow in the injected pulse and is suppressed at high CO2 flows. Relative to a conventional jet separator, the transmission efficiency of the axial jet separator is lower, but its performance is less sensitive to misalignments. PMID:26652049

  5. USAGE OF HYPHEN IN GEOLOGICAL REPORT%地质报告中连接号使用说明与辨析

    Institute of Scientific and Technical Information of China (English)

    刘伯崇

    2011-01-01

    本文阐述了6种形式的连接号的正确使用范围,并对连接号使用时最容易出现的混用和错误进行了辨析,以达到在编制地质报告运用连接号时避免误用混用的目的。%The essay expounded how to use hyphen in geological reports for 6 purposes,and discussed the common errors in using it.

  6. A Novel Combination of Immunoreaction and ICP-MS as a Hyphenated Technique for the Determination of Thyroid-stimulating Hormone (TSH) in Human Serum

    Institute of Scientific and Technical Information of China (English)

    2001-01-01

    The novel coupling method based on the hyphenation of immunoreaction with ICP-MS is developed and applied to the determination of thyroid-stimulating hormone (TSH) in human serum. In this system, TSH is firstly captured by anti-TSH monoclonal antibodies immobilized on a solid support. Biotinylated anti-TSH monoclonal antibodies and Eu3+-labelled streptavidin are then added to form the complex capturing andbody-TSH-biotinylated anti-TSH antibody-Eu3+-labeled streptavidin. After unbound reactants are washed away, Eu3+ bound to the complex is extracted by

  7. Micro solid phase spectrophotometry in a sequential injection lab-on-valve platform for cadmium, zinc, and copper determination in freshwaters.

    Science.gov (United States)

    Santos, Inês C; Mesquita, Raquel B R; Rangel, António O S S

    2015-09-01

    This work describes the development of a solid phase spectrophotometry method in a μSI-LOV system for cadmium, zinc, and copper determination in freshwaters. NTA (Nitrilotriacetic acid) beads with 60-160 μm diameter were packed in the flow cell of the LOV for a μSPE column of 1 cm length. The spectrophotometric determination is based on the colourimetric reaction between dithizone and the target metals, previously retained on NTA resin. The absorbance of the coloured product formed is measured, at 550 nm, on the surface of the NTA resin beads in a solid phase spectrophotometry approach. The developed method presented preconcentration factors in the range of 11-21 for the metal ions. A LOD of 0.23 μg L(-1) for cadmium, 2.39 μg L(-1) for zinc, and 0.11 μg L(-1) for copper and a sampling rate of 12, 13, and 15 h(-1) for cadmium, zinc, and copper were obtained, respectively. The proposed method was successfully applied to freshwater samples. PMID:26388376

  8. Recent developments in automated determinations of trace level concentrations of elements and on-line fractionations schemes exploiting the micro-sequential injection - lab-on-valve approach

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Miró, Manuel; Long, Xiangbao;

    2006-01-01

    are presented as based on the exploitation of micro-sequential injection (μSI-LOV) using hydrophobic as well as hydrophilic bead materials. The examples given comprise the presentation of a universal approach for SPE-assays, front-end speciation of Cr(III) and Cr(VI) in a fully automated and enclosed set...

  9. Lab-on-Valve Micro Sequential Injection: A Versatile Approach for Implementing Integrated Sample Pre-preparations and Executing (Bio)Chemical Assays

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    In the last decade, Flow Injection Analysis (FIA) became supplemented by Sequential Injection Analysis (SIA), which, although it inherently entails some limitations as compared to FIA, offers specific advantages, notably in terms of significantly reduced sample and reagent(s) consumption and henc...

  10. Lab-on-Valve Micro Sequential Injection: A Versatile Approach for Implementing Integrated Sample Pre-preparations and Executing (Bio)Chemical Assays

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    Since its introduction in 1975, Flow Injection Analysis (FIA) has established itself as an indispensable analytical concept that not only has permitted the implementation of numerous intriguing analysis procedures. But, more importantly, it has made it possible to facilitate the execution...

  11. Sensitive redox speciation of iron, neptunium, and plutonium by capillary electrophoresis hyphenated to inductively coupled plasma sector field mass spectrometry.

    Science.gov (United States)

    Graser, Carl-Heinrich; Banik, Nidhu Lal; Bender, Kerstin Anne; Lagos, Markus; Marquardt, Christian Michael; Marsac, Rémi; Montoya, Vanessa; Geckeis, Horst

    2015-10-01

    The long-term safety assessment for nuclear waste repositories requires a detailed understanding of actinide (geo)chemistry. Advanced analytical tools are required to gain insight into actinide speciation in a given system. The geochemical conditions in the vicinity of a nuclear repository control the redox state of radionuclides, which in turn has a strong impact on their mobility. Besides the long-lived radionuclides plutonium (Pu) and neptunium (Np), which are key elements in high level nuclear waste, iron (Fe) represents a main component in natural systems controlling redox-related geochemical processes. Measuring the oxidation state distribution for redox sensitive radionuclides and other metal ions is challenging at trace concentrations below the detection limit of most available spectroscopic methods (≥10(-6) M). Consequently, ultrasensitive new analytical techniques are required. Capillary electrophoresis (CE) is a suitable separation method for metal cations. CE hyphenated to inductively coupled plasma sector field mass spectrometry (CE-ICP-SF-MS) was used to measure the redox speciation of Pu (III, IV, V, VI), Np (IV, V, VI), and Fe (II, III) at concentrations lower than 10(-7) M. CE coupling and separation parameters such as sample gas pressure, make up flow rate, capillary position, auxiliary gas flow, as well as the electrolyte system were optimized to obtain the maximum sensitivity. We obtain detection limits of 10(-12) M for Np and Pu. The various oxidation state species of Pu and Np in different samples were separated by application of an acetate-based electrolyte system. The separation of Fe (II) and Fe (III) was investigated using different organic complexing ligands, EDTA, and o-phenanthroline. For the Fe redox system, a limit of detection of 10(-8) M was calculated. By applying this analytical system to sorption studies, we were able to underline previously published results for the sorption behavior of Np in highly diluted concentrations, and

  12. Sensitive redox speciation of iron, neptunium, and plutonium by capillary electrophoresis hyphenated to inductively coupled plasma sector field mass spectrometry.

    Science.gov (United States)

    Graser, Carl-Heinrich; Banik, Nidhu Lal; Bender, Kerstin Anne; Lagos, Markus; Marquardt, Christian Michael; Marsac, Rémi; Montoya, Vanessa; Geckeis, Horst

    2015-10-01

    The long-term safety assessment for nuclear waste repositories requires a detailed understanding of actinide (geo)chemistry. Advanced analytical tools are required to gain insight into actinide speciation in a given system. The geochemical conditions in the vicinity of a nuclear repository control the redox state of radionuclides, which in turn has a strong impact on their mobility. Besides the long-lived radionuclides plutonium (Pu) and neptunium (Np), which are key elements in high level nuclear waste, iron (Fe) represents a main component in natural systems controlling redox-related geochemical processes. Measuring the oxidation state distribution for redox sensitive radionuclides and other metal ions is challenging at trace concentrations below the detection limit of most available spectroscopic methods (≥10(-6) M). Consequently, ultrasensitive new analytical techniques are required. Capillary electrophoresis (CE) is a suitable separation method for metal cations. CE hyphenated to inductively coupled plasma sector field mass spectrometry (CE-ICP-SF-MS) was used to measure the redox speciation of Pu (III, IV, V, VI), Np (IV, V, VI), and Fe (II, III) at concentrations lower than 10(-7) M. CE coupling and separation parameters such as sample gas pressure, make up flow rate, capillary position, auxiliary gas flow, as well as the electrolyte system were optimized to obtain the maximum sensitivity. We obtain detection limits of 10(-12) M for Np and Pu. The various oxidation state species of Pu and Np in different samples were separated by application of an acetate-based electrolyte system. The separation of Fe (II) and Fe (III) was investigated using different organic complexing ligands, EDTA, and o-phenanthroline. For the Fe redox system, a limit of detection of 10(-8) M was calculated. By applying this analytical system to sorption studies, we were able to underline previously published results for the sorption behavior of Np in highly diluted concentrations, and

  13. High temperature liquid chromatography hyphenated with ESI-MS and ICP-MS detection for the structural characterization and quantification of halogen containing drug metabolites

    Energy Technology Data Exchange (ETDEWEB)

    Vlieger, Jon S.B. de [BioMolecular Analysis Group, Faculty of Sciences, VU University Amsterdam, De Boelelaan 1083, 1081 HV Amsterdam (Netherlands); Giezen, Mark J.N. [QPS Netherlands B.V., Petrus Campersingel 123, 9713 AG Groningen (Netherlands); Falck, David [BioMolecular Analysis Group, Faculty of Sciences, VU University Amsterdam, De Boelelaan 1083, 1081 HV Amsterdam (Netherlands); Tump, Cornelis; Heuveln, Fred van [QPS Netherlands B.V., Petrus Campersingel 123, 9713 AG Groningen (Netherlands); Giera, Martin; Kool, Jeroen; Lingeman, Henk [BioMolecular Analysis Group, Faculty of Sciences, VU University Amsterdam, De Boelelaan 1083, 1081 HV Amsterdam (Netherlands); Wieling, Jaap [QPS Netherlands B.V., Petrus Campersingel 123, 9713 AG Groningen (Netherlands); Honing, Maarten [DSM Resolve, PO Box 18, 6160 MD Geleen (Netherlands); Irth, Hubertus [BioMolecular Analysis Group, Faculty of Sciences, VU University Amsterdam, De Boelelaan 1083, 1081 HV Amsterdam (Netherlands); Niessen, Wilfried M.A., E-mail: W.M.A.Niessen@vu.nl [BioMolecular Analysis Group, Faculty of Sciences, VU University Amsterdam, De Boelelaan 1083, 1081 HV Amsterdam (Netherlands)

    2011-07-18

    Highlights: {yields} Hyphenation of high temperature liquid chromatography to ICP-MS and ESI-MS. {yields} Structural characterization of kinase inhibitor metabolites with high resolution MS{sup n} experiments. {yields} Quantification of drug metabolites with ICP-MS based on Iodine detection. {yields} Significant changes in ESI-MS response after small structural changes. - Abstract: In this paper we describe the hyphenation of high temperature liquid chromatography with ICP-MS and ESI-MS for the characterization of halogen containing drug metabolites. The use of temperature gradients up to 200 deg. C enabled the separation of metabolites with low organic modifier content. This specific property allowed the use of detection methods that suffer from (significant) changes in analyte response factors as a function of the organic modifier content such as ICP-MS. Metabolites of two kinase inhibitors (SB-203580-Iodo and MAPK inhibitor VIII) produced by bacterial cytochrome P450 BM3 mutants and human liver microsomes were identified based on high resolution MS{sup n} data. Quantification was done using their normalized and elemental specific response in the ICP-MS. The importance of these kinds of quantification strategies is stressed by the observation that the difference of the position of one oxygen atom in a structure can greatly affect its response in ESI-MS and UV detection.

  14. Inline roasting hyphenated with gas chromatography-mass spectrometry as an innovative approach for assessment of cocoa fermentation quality and aroma formation potential.

    Science.gov (United States)

    Van Durme, Jim; Ingels, Isabel; De Winne, Ann

    2016-08-15

    Today, the cocoa industry is in great need of faster and robust analytical techniques to objectively assess incoming cocoa quality. In this work, inline roasting hyphenated with a cooled injection system coupled to a gas chromatograph-mass spectrometer (ILR-CIS-GC-MS) has been explored for the first time to assess fermentation quality and/or overall aroma formation potential of cocoa. This innovative approach resulted in the in-situ formation of relevant cocoa aroma compounds. After comparison with data obtained by headspace solid phase micro extraction (HS-SPME-GC-MS) on conventional roasted cocoa beans, ILR-CIS-GC-MS data on unroasted cocoa beans showed similar formation trends of important cocoa aroma markers as a function of fermentation quality. The latter approach only requires small aliquots of unroasted cocoa beans, can be automatated, requires no sample preparation, needs relatively short analytical times (<1h) and is highly reproducible. PMID:27006215

  15. Analysis of the volatile oil from the stem of acanthopanax senticosus(Rupr.et Maxim.)harms with several hyphenated methods of chromatography

    Institute of Scientific and Technical Information of China (English)

    Yu Wanying; Zhang Hua; Huang Weidong; Chen Jiping; Liang Xinmiao

    2006-01-01

    Gas chromatography/quadrupole mass spectrometry (GC/qMS),gas chromatography/Fourier transform infrared spectrometry(CC/FTIR)and gas chromatography/orthogonal acceleration time-of-flight mass spectrometry(GC/oaTOFMS)were applied to analyze the volatile oil from the stem of Acanthopanax Senticosus(Rupr.et Maxim.)Harms.Based on the mass spectra search function of GC/qMS with the aid of the discriminability of the geometrical isomer by GC/FTIR and the ability to determine the accurate mass charge ratio(m/z)by GC/oaTOFMS,68 GC eluants were identified successfully.Compared with the results obtained by GC/qMS only,the analytical results obtained by these hyphenated methods of gas chromatography are more credible.

  16. The use of LC/MS, GC/MS, and LC/NMR hyphenated techniques to identify a drug degradation product in pharmaceutical development.

    Science.gov (United States)

    Pan, Changkang; Liu, Frances; Ji, Qin; Wang, Wei; Drinkwater, Donald; Vivilecchia, Richard

    2006-02-24

    Understanding drug degradation in the formulated product is critical in pharmaceutical development as it has significant impacts on drug efficacy, safety profile and storage conditions. As a result, identification of degradation compounds has taken an important role in the drug development process. In this study, various hyphenated analytical techniques, such as liquid chromatography mass spectrometry (LC/MS), gas chromatography mass spectrometry (GC/MS), and liquid chromatography nuclear magnetic resonance with a solid phase extraction interface (LC/SPE/NMR), have been applied to the identification of a drug degradation product which grew over time in the stability study of the drug product. The target unknown is less polar and more unsaturated than the drug substance based upon reverse phase HPLC relative retention time and UV spectra. It is not ionizable by electrospray ionization (ESI) or atmospheric pressure chemical ionization (APCI) in either a positive or a negative mode. The unknown was isolated by an HPLC fraction collector and enriched by solid phase extraction. GC/MS with chemical ionization (CI) was employed to determine the molecular weight of this compound. Its fragmentation pattern was determined by CI-MS/MS using an ion trap mass spectrometer. The isolated material was also analyzed by LC/SPE/NMR, from which the structure of this compound was further characterized. The study utilizes a combination of various hyphenated analytical techniques to obtain complimentary information for structure elucidation of the unknown. The combination approach is critical for unambiguous impurity structure elucidation in drug degradation studies of pharmaceutical drug products. PMID:16242883

  17. Mass spectrometry hyphenated techniques for the analysis of volatiles and peptides in soft cheese: Useful tools for the shelf life optimization.

    Science.gov (United States)

    Mentana, Annalisa; Natale, Anna; Palermo, Carmen; Nardiello, Donatella; Conte, Amalia; Del Nobile, Matteo Alessandro; Quinto, Maurizio; Centonze, Diego

    2016-07-01

    In order to assess the product quality and shelf life of an Italian soft cream cheese under different storage conditions, the volatile and peptide profiles evolution were tested. Volatiles were sampled directly from the head space of cheese packaging by solid-phase microextraction and analyzed by GC-MS. Peptide profiles were obtained by nanoLC-MS/MS, following a novel bioinformatics approach based on scoring distribution associated to the protein hits originating from the database search. In particular, a refined identification by focusing on selected time segments corresponding to the most intense peaks was carried out. A total of 40 compounds including acids, aldehydes, ketones, lactones, alcohols, esters, hydrocarbons, terpene, sulfur, and aromatic compounds were detected. Significant differences in their abundance during the storage in different packagings were observed, as well as an evolution of peptides mainly belonging to αS1-casein. The results demonstrated the usefulness of the above-mentioned hyphenated techniques for the determination of the soft cheese shelf life under different storage conditions. PMID:26800207

  18. Research Progress in the Speciation of Arsenic with Hyphenated Techniques%联用技术在砷形态分析中的研究进展

    Institute of Scientific and Technical Information of China (English)

    李林林; 朱英存

    2013-01-01

    Currently the main analysis techniques for arsenic speciation were the combination of chromatograph with atomic spectrum and mass spectrum, especially the combination of HPLC with ICP-OES or ICP-MS. The methods were accurate and reliable and had high sensitivity. But they can not provide the structural information of arsenic compounds. So the combination of chromatograph with ESI-MS was used as the main method for qualitative analysis. The insufficient sensitivity and vulnerability to matrix interference of ESI-MS can be overcome by the complex pretreatment technique. In this article hyphenated techniques were evaluated with particular emphasis on interfaced separation with element-selective detection and identification of the arsenic compounds detected.%  目前用元素砷的形态分析技术主要是色谱与子光谱、质谱等的联用,最常用的是HPLC与ICP-OES、 ICP-MS的联用,方法准确可靠,灵敏度高,但是不能提供砷化合物的分子结构信息。此以色谱-电喷雾质谱(ESI-MS)的联用作为定性分析的主要手段,但是ESI-MS灵敏度低,易受基体干扰,此需要复杂的前处理技术。

  19. 联用色谱完全重叠峰的解析方法%Resolution Methods of Hyphenated Embedded Chromatographic Peaks

    Institute of Scientific and Technical Information of China (English)

    陈迪钊; 毛新平

    2000-01-01

    Based on orthogonal projection technique and constrained peak shape condition, three kind of new methods to resolve completely overalapping chromatographic peaks are proposed in this paper. They are constrained peak shape and curve fitting resolution(CPSCF), iterative orthogonal projection resolution(IOP) and rank annihilation factor analysis(RAFA). If the constrain conditions is satisfied on hyphenated chromatography data matrics, these methods can be proved to be completely possible for them to be used on the resolution of spectra for embedded and concentration profiles for embedding peaks.%基于正交投影技术和约束峰形条件,本文提出了三种完全重叠色谱峰的解析方法,峰形约束曲线拟合解析(CPSCF),交替正交投影(IOP)和秩消失因子分析(RAFA)。对联用色谱数据阵如果约束条件得到满足,这些方法能被证明用于被嵌人组分的光谱和嵌入组分的浓度曲线分辨是完全可能地。

  20. 联用技术在砷形态分析中的研究进展%Research Progress in the Speciation of Arsenic with Hyphenated Techniques

    Institute of Scientific and Technical Information of China (English)

    李林林; 朱英存

    2013-01-01

    Currently the main analysis techniques for arsenic speciation were the combination of chromatograph with atomic spectrum and mass spectrum, especially the combination of HPLC with ICP-OES or ICP-MS. The methods were accurate and reliable and had high sensitivity. But they can not provide the structural information of arsenic compounds. So the combination of chromatograph with ESI-MS was used as the main method for qualitative analysis. The insufficient sensitivity and vulnerability to matrix interference of ESI-MS can be overcome by the complex pretreatment technique. In this article hyphenated techniques were evaluated with particular emphasis on interfaced separation with element-selective detection and identification of the arsenic compounds detected.%  目前用元素砷的形态分析技术主要是色谱与子光谱、质谱等的联用,最常用的是HPLC与ICP-OES、 ICP-MS的联用,方法准确可靠,灵敏度高,但是不能提供砷化合物的分子结构信息。此以色谱-电喷雾质谱(ESI-MS)的联用作为定性分析的主要手段,但是ESI-MS灵敏度低,易受基体干扰,此需要复杂的前处理技术。

  1. Physicochemical characterization of titanium dioxide pigments using various techniques for size determination and asymmetric flow field flow fractionation hyphenated with inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Helsper, Johannes P F G; Peters, Ruud J B; van Bemmel, Margaretha E M; Rivera, Zahira E Herrera; Wagner, Stephan; von der Kammer, Frank; Tromp, Peter C; Hofmann, Thilo; Weigel, Stefan

    2016-09-01

    Seven commercial titanium dioxide pigments and two other well-defined TiO2 materials (TiMs) were physicochemically characterised using asymmetric flow field flow fractionation (aF4) for separation, various techniques to determine size distribution and inductively coupled plasma mass spectrometry (ICPMS) for chemical characterization. The aF4-ICPMS conditions were optimised and validated for linearity, limit of detection, recovery, repeatability and reproducibility, all indicating good performance. Multi-element detection with aF4-ICPMS showed that some commercial pigments contained zirconium co-eluting with titanium in aF4. The other two TiMs, NM103 and NM104, contained aluminium as integral part of the titanium peak eluting in aF4. The materials were characterised using various size determination techniques: retention time in aF4, aF4 hyphenated with multi-angle laser light spectrometry (MALS), single particle ICPMS (spICPMS), scanning electron microscopy (SEM) and particle tracking analysis (PTA). PTA appeared inappropriate. For the other techniques, size distribution patterns were quite similar, i.e. high polydispersity with diameters from 20 to >700 nm, a modal peak between 200 and 500 nm and a shoulder at 600 nm. Number-based size distribution techniques as spICPMS and SEM showed smaller modal diameters than aF4-UV, from which mass-based diameters are calculated. With aF4-MALS calculated, light-scattering-based "diameters of gyration" (Øg) are similar to hydrodynamic diameters (Øh) from aF4-UV analyses and diameters observed with SEM, but much larger than with spICPMS. A Øg/Øh ratio of about 1 indicates that the TiMs are oblate spheres or fractal aggregates. SEM observations confirm the latter structure. The rationale for differences in modal peak diameter is discussed.

  2. Home-made online hyphenation of pressurized liquid extraction, turbulent flow chromatography, and high performance liquid chromatography, Cistanche deserticola as a case study.

    Science.gov (United States)

    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.

  3. Analysis of tetrodotoxin by hyphenated chromatographic techniques%多种色谱联用技术分析替曲朵辛

    Institute of Scientific and Technical Information of China (English)

    代秀梅; 于风平; 张启明

    2013-01-01

    目的:建立替曲朵辛原料药含量及有关物质的测定方法,并对有关物质的结构进行分析.方法:采用HPLC法测定替曲朵辛原料药含量及有关物质,采用UPLC-UV-MS/MS和LC-NMR联用技术对含量最高的杂质9的结构进行分析.结果:重复性好,替曲朵辛浓度在0.294~44.16 μg· mL-1范围内线性关系良好(r =0.9999),有关物质中最大杂质为4,9,10,11二脱水河豚毒素.结论:本方法操作简便,结果准确,可作为替曲朵辛原料药含量测定和有关物质检查的方法.%Objective:To establish a hyphenated chromatographic method for content determination of tetrodotoxin (TTX) raw medicine and related substances and to analyze the structure of related substances.Methods:HPLC was used to determin the content of tetrodotoxin mw medicine and related substances,and UPLC-UV-MS/MS and LC-NMR were used to study the structure of related substances.Results:There was a good linear relationship for tetrodotoxin in the range of 0.294-44.16 μg · mL-1 (r =0.9999).The impurity of the highest content was 4,9,10,11-dianhydro-TTX.Conclusion:The method is simple,accurate,and well reproducible which can be applied to content determination of Tet rodotoxin raw medicine and related substances.

  4. Speciation of the bio-available iodine and bromine forms in edible seaweed by high performance liquid chromatography hyphenated with inductively coupled plasma-mass spectrometry

    International Nuclear Information System (INIS)

    Highlights: ► Bioavailable iodine and bromine speciation in edible seaweed were developed. ► In vitro dialyzability was used to assess the bioavailable fractions. ► AEC hyphenated with inductively coupled plasma-mass spectrometry was used. ► Iodide, MIT, DIT, bromide and bromate were found in dialyzates from edible seaweed. ► Positive correlation between bioavailability and protein contents was found. - Abstract: A bioavailability study based on an in vitro dialyzability approach has been applied to assess the bio-available fractions of iodine and bromine species from edible seaweed. Iodide, iodate, 3-iodo-tyrosine (MIT), 3,5-diiodo-tyrosine (DIT), bromide and bromate were separated by anion exchange chromatography under a gradient elution mode (175 mM ammonium nitrate plus 15% (v/v) methanol, pH 3.8, as a mobile phase, and flow rates within the 0.5–1.5 mL min−1 range). Inductively coupled plasma-mass spectrometry (ICP-MS) was used as a selective detector for iodine (127I) and bromine (79Br). Low dialyzability ratios (within the 2.0–18% range) were found for iodine species; whereas, moderate dialyzability percentages (from 9.0 to 40%) were obtained for bromine species. Iodide and bromide were the major species found in the dialyzates from seaweed, although MIT and bromate were also found in the dialyzates from most of the seaweed samples analysed. However, DIT was only found in dialyzates from Wakame, Kombu, and NIES 09 (Sargasso) certified reference material; whereas, iodate was not found in any dialyzate. Iodine dialyzability was found to be dependent on the protein content (negative correlation), and on the carbohydrate and dietary fibre levels (positive correlation). However, bromine dialyzability was only dependent on the protein amount in seaweed (negative correlation).

  5. Hyphenated LC-MALDI-ToF/ToF and LC-ESI-QToF approach in proteomic characterization of honeybee venom.

    Science.gov (United States)

    Matysiak, Jan; Hajduk, Joanna; Mayer, Franz; Hebeler, Romano; Kokot, Zenon J

    2016-03-20

    To increase in the depth characterization of venom proteome of Apis mellifera the hyphenated LC-MALDI-ToF/ToF-MS (liquid chromatography-matrix-assisted laser desorption/ionization-time of flight/time of flight tandem mass spectrometry) and LC-ESI-QToF-MS (liquid chromatography-electrospray ionization-quadrupole time of flight tandem mass spectrometry) techniques combined with combinatorial peptide ligand library enrichment method is proposed in this study. The novel approach simplifies pretreatment protocol in venom investigation. By using the protein preparation kit with sequential multi-step elution, the honeybee venom was dispensed into four different fractions. In total 269 proteins were detected, among these 49 honeybee toxins, allergens and components involved in mechanism of envenoming belonging to venom enzyme classes of esterases, proteases/peptidases, protease inhibitors, hydrolases and major royal jelly proteins. Moreover 5 additional putative toxins were identified. Their role in envenoming process was discussed. We concluded that different mass spectrometry techniques increased the detection of the honeybee venom proteins, underscoring the complementary character of analytical methods. The combination of MALDI and ESI ionization has resulted in numerous proteins identifications, not possible to reach with single proteomic technique. The study will contribute to broadening the knowledge about the complexity of honeybee venom. The newly identified proteins may serve not only as toxins and allergens, but also as substances with potential pharmacological activity. Although, the most detected proteins belong to trace elements of honeybee venom without toxic activity or action on vital system of victims, they should be taken into account in characterization of living organism response on Apis mellifera sting. PMID:26780156

  6. Solid reactors in sequential injection analysis: Recent trends in the environmental field

    DEFF Research Database (Denmark)

    Miró, Manuel; Hansen, Elo Harald

    2006-01-01

    The second generation of flow injection analysis (FIA), so-called sequential injection (SI), has already been consolidated as an attractive flowing-stream approach in several analytical fields, with advantages over the first generation of FIA in terms of automation, miniaturization, and sample...... applications, aiming to facilitate on-line chemical derivatization, chromatographic separation of target species, removal of interfering matrix compounds, or determination of trace levels of analyte via sorptive preconcentration procedures. In this context, the concept of renewable surfaces, so-called SI......-bead injection (SI-BI), used in either the jet-ring or lab-on-valve configurations, is presented as a front-end to many detectors. This article also outlines recent trends focused on exploiting SI as an automated tool for handling solid samples of environmental concern and accommodating dynamic fractionation...

  7. 盐酸法舒地尔有关物质的色谱-质谱结构鉴定%Identification of the related substances in fasudil hydrochloride with hyphenated techniques

    Institute of Scientific and Technical Information of China (English)

    陈月琴; 宋敏; 杭太俊

    2013-01-01

    The study aims to identify the related substances in fasudil hydrochloride by hyphenated techniques. A WondaSil C18 (250 mm × 4.6 mm, 5 μm) column was used for the separation of the related substances with a mixture of methanol and ammonium acetate buffer solution as the mobile phase by gradient elution. The structures of the related substances were speculated by electrospray positive ionization LC-TOF/ MS accurate ion mass and MS/MS determination and elucidation, and verified further through synthesis and spectroscopic analysis. Fasudil hydrochloride and the related substances were separated under the established HPLC condition. Three related substances in fasudil hydrochloride were characterized by hyphenated techniques. The hyphenated LC-MS method is useful for the identification of related substances in fasudil hydrochloride and the results obtained are valuable for its manufacturing process and quality control.%采用WondaSil C18 (250 mm×4.6 mm ID,5 μm)色谱柱,甲醇-醋酸铵缓冲溶液流动相梯度洗脱,对盐酸法舒地尔有关物质进行分离;采用正离子电喷雾-飞行时间质谱法测定准确质量和二级串联质谱分析离子结构特征,并结合合成制备与波谱解析确证主要有关物质结构.结果显示,盐酸法舒地尔与其有关物质分离良好,检测出3个主要有关物质,并综合分析鉴定了有关物质结构.色谱-质谱联用技术能有效地鉴定盐酸法舒地尔有关物质,为其工艺和质量控制提供参考依据.

  8. 中英文破折号、连接号用法异同比较%Similarities and Differences of Usage between Chinese and English Punctuation of Dash/Hyphen

    Institute of Scientific and Technical Information of China (English)

    马奋华; 倪东鸿; 王小曼

    2006-01-01

    针对科技论文中中文破折号、连接号与英文破折号(dash)、连字号(hyphen)用法混乱的现象,参考有关国家标准、文献和国外优秀期刊的编辑规范,指出了4个标点符号的具体表现形式和用法,以及应用中注意的问题,并提出了相应的修改意见,以期引起同行和有关权威部门的重视,达到规范应用这4个标点符号的目的.

  9. 超临界流体分离与NMR联用技术及其应用%Hyphenation of Supercritical Fluid Separation with Nuclear Mag netic Resonance and Their Applications

    Institute of Scientific and Technical Information of China (English)

    陈志伟; 陈忠

    2001-01-01

    The progression,instruments and applications of hyphenation between supercritica l fluid separation (SFC or SFE) and NMR spectrometry were described.The resoluti on of 1H NMR spectra obtained in SFC-NMR and SFE-NMR experiments is compared with that obtained by HPLC-NMR experiments. This review also looks for ward to the future of SFC-NMR and SFE-NMR.%本文重点描述了SFC-NMR和SFE-NMR联用装置的特点及其探头设计,举例说明了它们的几种典型应用,分析比较了超临界流体分离和NMR联用系统与HPLC-NMR联 用系统的特性,并讨论了超临界流体分离与NMR联用技术的发展前景。

  10. Application of microdialysis and its hyphenated techniques in studies of traditional Chinese medicines%微透析及其联用技术在中药研究中的应用

    Institute of Scientific and Technical Information of China (English)

    曹柳; 辛贵忠; 闻晓东; 李萍

    2012-01-01

    微透析技术是用于监测细胞外液中内源性物质及外源性物质的活体取样技术,但由于微透析样品是一种含有高浓度无机盐的复杂混合物,往往需要与色谱分离技术联合使用,才能对微透析样品中目标分析物进行测定.目前,微透析与高分辨率、高灵敏度的分析技术的联用已得到广泛应用,该技术的应用,为现代中药的研究提供了一种新的思路和工具.本文概述了微透析技术的原理及特点,重点介绍了微透析及其联用技术在中药干预下内源性物质的分析、中药药代动力学及相互作用研究中的应用..%Microdialysis (MD) is an in vivo technique used for sampling endogenous and exogenous substances in the extracellular space. However, MD samples are complex mixtures containing high concentrations of inorganic salts that require chromatographic separation to allow for the measurements of interest analytes. Currently, MD combined with high resolution and sensitivity analytical techniques have been used widely. MD and its hyphenated techniques provide new ideas and tools for research of traditional Chinese medicines (TCMs). This review summarized the principles and characteristics of MD techniques, and focused on the applications of MD and its hyphenated techniques in the analysis of endogenous substances, pharmacokinetic study of TCMs and herbs-drug interactions.

  11. Off-line hyphenation of boronate affinity monolith-based extraction with matrix-assisted laser desorption/ionization time-of-flight mass spectrometry for efficient analysis of glycoproteins/glycopeptides.

    Science.gov (United States)

    Bie, Zijun; Chen, Yang; Li, Hengye; Wu, Ronghu; Liu, Zhen

    2014-06-27

    Boronate affinity materials have attracted increasing attentions as sample enrichment platforms for glycoproteomic analysis in recent years. However, most of the boronate affinity materials that have already employed for proteomic analysis are suffering from apparent disadvantages, such as alkaline pH for binding, weak affinity, and relatively poor selectivity. Benzoboroxoles are a unique class of boronic acids which have showed excellent binding properties for the recognition of cis-diol-containing compounds. Recently, a 3-carboxy-benzoboroxole-functionalized monolithic column had been reported and it had exhibited the best selectivity and affinity as well as the lowest binding pH among all reported boronate affinity monolithic columns. In this study, an off-line hyphenation of this boronate affinity monolithic column-based extraction with matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) was developed and the powerfulness of this hyphenated approach in the analysis of glycoproteins and glycopeptides in complex samples was investigated. The approach was first applied to the analysis of glycopeptides in the tryptic digest of horseradish peroxidase (HRP). Totally 22 glycopeptides were identified. To the best of our knowledge, this is the best performance among all the boronic acid-functionalized materials. We further employed this approach to the analysis of intact proteins in human saliva. Totally 6 intact glycoproteins were successfully identified. As comparison, when the samples were analyzed without extraction, only a few glycopeptides were identified from the tryptic digest of HRP while no glycoproteins were found from the saliva samples. PMID:24928239

  12. 介观(微)流控分析技术:第三代流动注射分析--阀上实验室%MESO-MICROFLUIDICS CONTROL TECHNIQUE: LAB-ON-VALVE--THE THIRD GENERATION OF FLOW INJECTION

    Institute of Scientific and Technical Information of China (English)

    王建华; 方肇伦

    2003-01-01

    @@ 1 Micro total analysis (μTAS) system vs the three generations of flow injection Appropriate sample pretreatment prior to analysis remains inevitably the bottle neck of the entire analytical procedure with modern instrumentation[1],where flow injection analysis (FIA) has led to sig nificant progress. Flow injection (FI) and sequential injection (SI),termed as the first and the second generations of FIA,have played important roles in the automation and miniaturization of on-line sample pretreatment[2]. While in further downscaling of fluidic control ,the micro total analysis system (μTAS)has drawn considerable attention[3].

  13. Determination of trace metal ions via on-line separation and preconcentration by means of chelating Sepharose beads in a sequential injection lab-on-valve (SI-LOV) system coupled to electrothermal atomic absorption spectrometric detection

    DEFF Research Database (Denmark)

    Long, Xiangbao; Hansen, Elo Harald; Miró, Manuel

    2005-01-01

    . The samples are adjusted to pH 5.0 on-line in the system for optimum operation. The target ions are adsorbed by chelation on the surface of the beads, contained in a 20 mul microcolumn within the LOV, and following elution by 50 mul 2M nitric acid, the eluate is, as sandwiched by air segments, introduced...

  14. Evaluation of a novel PTFE material for separation and preconcentration of trace levels of metal ions in sequential injection (SI) and sequential injection lab-on-valve (SI-LOV) systems interfaced with detection by ETAAS

    DEFF Research Database (Denmark)

    Long, Xiangbao; Chomchoei, Roongrat; Gała, Piotr;

    The operational characteristics of a novel PTFE bead material, granular Algoflon®, used for separation and preconcentration of metal ions via adsorption of on-line generated non-charged metal complexes, were evaluated in a sequential injection (SI) system furnished with an external packed column...

  15. Highly selective micro-sequential injection lab-on-valve (μSI-LOV) method for determination of ultra trace concentrations of nickel in saline matrices using detection by electrothermal atomic absorption spectrometr

    DEFF Research Database (Denmark)

    Long, Xiangbao; Miró, Manuel; Jensen, Rikard;

    2006-01-01

    methodology showed high tolerance to the commonly encountered alkaline earth matrix elements in environmental waters, that is, calcium and magnesium, and was successfully applied for the determination of nickel in an NIST standard reference material (NIST 1640-Trace elements in natural water), household tap...... water of high hardness and local seawater. Satisfying recoveries were achieved for all spiked environmental water samples with maximum deviations of 6%. The experimental results for the standard reference material were not statistically different to the certified value at a significance level of 0.05....

  16. On-line ion exchange preconcentration in a sequential injection lab-on-valve microsystem incorporating a renewable column with ETAAS for the trace-level determination of bismuth in urine and river sediment

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2001-01-01

    A sequential injection system for on-line ion-exchange separation and preconcentration of trace-level amounts of metal ions with ensuing detection by electrothermal atomic absorption spectrometry (ETAAS) is described. Based on the use of a renewable microcolumn incorporated within an integrated l.......3% for the determination of 2.0 mug/l Bi (n = 7). The procedure was validated by determination of bismuth in a certified reference material CRM 320 (river sediment), and by bismuth spike recoveries in two human urine samples....

  17. 富马酸替诺福韦双特戊酯有关物质的鉴定%Identification of the related substances in tenofovir dipivoxil fumarate with hyphenated techniques

    Institute of Scientific and Technical Information of China (English)

    赵画; 宋敏; 杭太俊

    2012-01-01

    目的:采用色谱-质谱联用技术对富马酸替诺福韦双特戊酯中有关物质进行结构鉴定.方法:采用BDS Hypersil C18(250 mm×4.6 mm,5μm)色谱柱,流动相为乙腈-0.2%醋酸铵溶液,梯度洗脱,对富马酸替诺福韦双特戊酯有关物质进行分离;LC-PDA测定各有关物质的UV吸收,甲醇辅助电喷雾正离子化LC-TOF和LC-MS/MS分别测定各有关物质的精密质量和二级质谱.结果:检测到富马酸替诺福韦双特戊酯中存在多个有关物质,其中仅3个的含量在0.1%以上,并鉴定出4个主要有关物质的结构.结论:色谱-质谱联用技术能够有效地鉴定药物中的有关物质,富马酸替诺福韦双特戊酯有关物质鉴定结果对其质量控制和工艺优化提供了参考依据.%Objective:To identify the related substances in tenofovir dipivoxil fumarate by hyphenated techniques. Methods: An LC-PDA-MS/MS method was established by using acetonitrile-O. 2% ammonium acetate as the mobile phase with gradient elution on a BDS Hypersil C18 (250 mm × 4. 6 mm,5 μm) column with 0. 2 mL-min methanol aided electro-spray positive ionization. The UV spectrum, accurate molecular weight and formula, and product ion MS spectrum of each related substance was obtained by LC-PDA ,LC-TOF and LC-MS/MS,respectively. Results: Several related substances were found in tenofovir dipivoxil fumarate with only 3 of them had the area normalization content over 0. 1% , and 4 of them were identified and elucidated. Conclusion: The hyphenated LC-MS method is useful for the determination and identification of related substances in pharmaceuticals. Identification of the related compounds in tenofovir dipivoxil fumarate is valuable for its manufacturing process optimization and quality control.

  18. Application Progresses on SFE-MD Hyphenated Techniques in the Separation and Purification of Nature Products%SFE-MD联用技术在天然产物分离提纯中的应用进展

    Institute of Scientific and Technical Information of China (English)

    狄崇耀; 李霞; 狄红旗

    2012-01-01

    分子蒸馏技术与超临界萃取技术都是新型的绿色分离技术,二者联用技术也一直备受各国关注。本文介绍了超临界萃取(SFE)与分子蒸馏(MD)技术的原理特点,综合评述了SFE-MD联用技术在天然产物分离提纯中的发展概况及其应用特点,并对该技术在天然产物提纯方面的前景进行了展望。%Technique of molecular distillation and supercritical extraction technology were the new types of green separation technology,and their hyphenated techniques were also concerned in all countries.Characteristics of the supercritical fluid extraction(SFE)and molecular distillation(MD) technique,and the developments and application characteristics of SFE-MD combination technology in the separation and purification of natural products,were introduced and the technology in the purification of natural products was prospected.

  19. Usages of Dashes and Hyphens in English Scientific Papers%英文科技出版物中横线类标点符号用法辨析

    Institute of Scientific and Technical Information of China (English)

    曾晓梅

    2011-01-01

    英语书刊中横线类标点符号,常用的包括em dash(破折号),en dash(连接号),hyphen(连字符)等,出错情况较多.疏误主要表现在不区分各符号间的差异以及与相应中文符号混用.em dash,en dash,hyphen与中文-字线和半字线相混淆的情况很普遍.这几个符号形状不同,语法意义也不-样.根据编辑实践中遇到的问题及相关丈献,对英文横线类标点符号的用法进行了归纳和分析,旨在提醒同行在编辑校对时加以注意.

  20. Study on multielemental speciation analysis of Cr(VI), As(III) and As(V) in water by advanced hyphenated technique HPLC/ICP-DRC-MS. Fast and reliable procedures.

    Science.gov (United States)

    Marcinkowska, Monika; Komorowicz, Izabela; Barałkiewicz, Danuta

    2015-11-01

    Analytical procedures for multielemental speciation analysis of arsenite - As(III), arsenate - As(V) and hexavalent chromium - Cr(VI) in water using high performance liquid chromatography inductively coupled plasma mass spectrometry (HPLC/ICP-DRC-MS) hyphenated technique have been developed. A dynamic reaction cell (DRC) for spectral interferences elimination has been involved in the experiment. Application of oxygen and ammonia as reaction gases in the DRC under various conditions has been verified. Optimization of the following chromatographic conditions: mobile phase composition, concentration of particular components, mobile phase pH and flow rate, injection volume and column temperature, has been conducted. Species separation has been carried out on anion-exchange chromatographic column using isocratic elution with: 22 mM (NH4)2HPO4, 25 mM NH4NO3 (for procedure A) and 22 mM (NH4)2HPO4, 65 mM NH4NO3 (for procedure B) as mobile phases. Detection limits (LD) for procedure A were 0.16 µg L(-1), 0.090 µg L(-1), 0.073 µg L(-1), and for procedure B were 0.14 µg L(-1), 0.062 µg L(-1), 0.15 µg L(-1) for As(III), As(V) and Cr(VI), respectively. Linearity was tested at two concentration ranges of: (0.5-10.0) µg L(-1) for procedure A and (5-50) µg L(-1) for procedure B, and showed correlation coefficients for each of the analytes to be above 0.999. Repeatability values obtained for spiked real water samples were in the range of (4.2-7.6)% and (2.0-2.4)% for procedure A and B respectively. Accuracy was calculated based on the analysis of spiked real water samples at three concentration levels. Obtained recoveries were from 94% to 102%. PMID:26452815

  1. Hyphenation of a EC / OC thermal-optical carbon analyzer to photo ionization time-of-flight mass spectrometry: a new off-line aerosol mass spectrometric approach for characterization of primary and secondary particulate matter

    Directory of Open Access Journals (Sweden)

    J. Diab

    2015-01-01

    Full Text Available Source apportionment and exposure of primary and secondary aerosols remains a challenging research field. In particular, the organic composition of primary particles and the formation mechanism of secondary organic aerosols (SOA warrant further investigations. Progress in this field is strongly connected to the development of novel analytical techniques. In this study an off-line aerosol mass spectrometric technique based on filter samples, a hyphenated thermal/optical analyzer-photo ionization time of flight mass spectrometer (PI-TOFMS system, was developed. The approach extends the capability of the widely used PM carbon analysis (for elemental/organic carbon (EC / OC by enabling the investigation of evolved gaseous species with soft and selective (resonance enhanced multiphoton ionization, REMPI and non-selective photo ionization (single photon ionization, SPI techniques. SPI was tuned to be medium soft to achieve comparability with results obtained by electron ionization (EI aerosol mass spectrometer (AMS. Different PM samples including wood combustion emission samples, smog chamber samples from the reaction of ozone with different SOA precursors, and ambient samples taken at Ispra, Italy in winter as well as in summer were tested. The EC / OC-PI-TOFMS technique increases the understanding of the processes during the thermal/optical analysis and identifies marker substances for the source apportionment. Composition of oligomeric or polymeric species present in PM can be investigated by the analysis of the thermally breakdown products. In case of wood combustion, in addition to the well-known markers at m/z ratios of 60 and 73, two new characteristic masses (m/z 70 and 98 have been revealed as potentially linked to biomass burning. All four masses were also the dominant signals in an ambient sample taken in winter time in Ispra, Italy, confirming the finding that wood burning for residential heating is a major source for particulate matter

  2. 气相色谱与热解吸联用技术在室内环境检测领域的应用及进展%Application and Development of Gas Chromatography Hyphenated with Thermal Desorption in the Field of Indoor Environment Testing

    Institute of Scientific and Technical Information of China (English)

    贾祥焱

    2012-01-01

    It is a brief introduction of gas chromatography and the application and development of gas chromatography hyphenated with thermal desorption in the test benzene and TVOC of indoor environment testing,and puts forward outlook and prospect in it.It provides favorable value in the development of gas chromatographic technique in indoor environment testing.%简要介绍了气相色谱法,及其与热解吸联用在民用建筑工程室内环境检测中检测苯、TVOC的应用和进展。并提出了气相色谱与热解吸联用技术的前景与展望,为气相色谱技术在室内环境检测领域的发展提供有利价值。

  3. HPLC-ICP/MS联用同时分析中药材中的多种形态砷%Analysis of arsenic speciation in traditional Chinese medicines by hyphenated technique of high performance liquid chromatography-inductively coupled plasma mass spectrometry

    Institute of Scientific and Technical Information of China (English)

    郝春莉; 赵丽; 庄峙厦

    2011-01-01

    The hyphenated technique of high performance liquid chromatography coupled with inductively coupled plasma-mass spectrometry (HPLC-ICP-MS) were applied in the simultaneous determination of six arsenic species including As( Ⅲ ) 、As( Ⅴ ) 、DMA、MMA、AsB and AsC, in traditional Chinese medicines. The arsenic species in Traditional Chinese Medicinal samples were extracted using 1.2 mol/L hydrochloric acid and analyzed by the hyphenated technique of HPLC-ICP-MS with Hamilton PRP-X100 column. The arsenic species were separated well in the 800s,and the detection limits were 0. 2 ~ 0. 6 μg. Arsenate As(Ⅴ) and arsenite As(Ⅲ) were main arsenic species in all samples,and the inorganic arsenic recoveries were 64%. 1% ~91.7%. In addition, a little arsenobetaine (AsB) was found in animal herbs. The method can be applied to the quantitative determination and safety evaluation of inorganic arsenic or six arsenic species in TCMs.%利用高效液相色谱-电感耦合等离子体质谱(HPLC-ICP/MS)对中药材中的6种砷的形态(三价砷(As(Ⅲ))、五价砷(As(Ⅴ))、二甲基砷酸(DMA)、甲基砷酸(MMA)、砷甜菜碱(AsB)和砷胆碱(AsC))进行了同时分析.采用1.2mol/,L HCl浸提,Hamilton PRP-X100阴离子交换色谱柱分离后,根据ICP/MS保留时间的差别跟踪检测砷元素的各种形态.6种砷形态在800s内分离良好,检测限在0.2~0.6μg/L之间;中药材中的砷主要以有毒的无机砷(As(Ⅴ)和As(Ⅲ))形态存在,样品中无机砷的回收率在64.1%~91.7%之间,另外动物药材中还存在微量的AsB等有机砷形态.方法可用于中药材中无机砷或各种砷形态的同时分析.

  4. Hyphenated Technique of Anti Asthma Application of Chemical Drugs Added Illegally in Traditional Chinese Medicine in the Identification%色谱联用技术在鉴定抗哮喘中药制剂中非法添加化学药物的应用

    Institute of Scientific and Technical Information of China (English)

    付蔷

    2014-01-01

    Traditional Chinese medicine to medication safety,become a common clinical drug treatment of asthma. In recent years,Chinese medicine clinical treatment of asthma often found il egal y mixed into chemical drug ingredients,pose a serious threat to patient safety.This paper reviews the application of hyphenated chromatographic techniques in the identification of chemical drugs added il egal y anti asthma in Chinese medicine preparation,in order to provide reference for the clinical detection.%中药制剂以其安全可靠的用药特点,成为临床治疗哮喘的常用药物。近年来,临床治疗哮喘的中药制剂中经常发现非法掺入化学类药物成分,给患者的用药安全带来严重威胁。本文分析了色谱联用技术在鉴定抗哮喘中药制剂中非法添加化学药物的应用进展,以期为临床检测提供参考。

  5. Separation and preconcentration of ultratrace levels of cadmium(II) in a sequential injection (SI) system with a PTFE packed column as a mimic sequential injection lab-on-valve (SI-LOV) system with renewable column employing detection by electrothermal atomic absorption spectrometry (ETAAS)

    DEFF Research Database (Denmark)

    Long, Xiangbao; Chomchoei, Roongrat; Gała, Piotr;

    cadmium(II) by detection with electrothermal atomic absorption spectrometry (ETAAS). The non-charged complex formed between the analyste and the chelating reagent diethyldithiophosphate (DDPA) was selectively adsorbed on the surface of the PTFE beads and eluted by ethanol before being directed to the...

  6. Evaluation of a novel PTFE material for use as a means for separation and preconcentration of trace levels of metal ions in sequential injection (SI) and sequential injection lab-on-valve (SI-LOV) systems. Determination of cadmium (II) with detection by electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Long, Xiangbao; Chomchoei, Roongrat; Hansen, Elo Harald;

    2004-01-01

    The operational characteristics of a novel poly(tetrafluoroethylene) (PTFE) bead material, granular Algoflon®, used for separation and preconcentration of metal ions via adsorption of on-line generated non-charged metal complexes, were evaluated in a sequential injection (SI) system furnished...

  7. Direct 13C NMR Detection in HPLC Hyphenation Mode

    DEFF Research Database (Denmark)

    Wubshet, Sileshi Gizachew; Johansen, Kenneth; Nyberg, Nils;

    2012-01-01

    Solid phase extraction (SPE) was introduced as a crucial step in the HPLC-SPE-NMR technique to enable online analyte enrichment from which proton-detected NMR experiments on submicrogram amounts from complex mixtures were possible. However, the significance of direct-detected (13)C NMR experiments...... application of HPLC-SPE-NMR analysis using direct-detected (13)C NMR spectra. HPLC column loading, accumulative SPE trappings, and the effect of different elution solvents were evaluated and optimized. A column loading of approximately 600 mug of a prefractionated triterpenoid mixture, six trappings...

  8. 谈谈英文标点dash与hyphen

    Institute of Scientific and Technical Information of China (English)

    黎秋萍; 金丽莉

    2004-01-01

    @@ 现在国人用英文写作(学术著作、论文等)已经比较普遍,涉及英语的报刊、教学材料、阅读辅导书更是不断出版.但是编著者往往不太注意英语书写中标点符号的使用规则.虽然中英文标点符号的功能大同小异,然而这个"小异"却不可忽视.据笔者掌握的情况,误用率最高的当属dash与hyphen了.为了让读者对它们有个感性认识,首先请看下面所列的表.

  9. Smart thorium and uranium determination exploiting renewable solid-phase extraction applied to environmental samples in a wide concentration range.

    Science.gov (United States)

    Avivar, Jessica; Ferrer, Laura; Casas, Montserrat; Cerdà, Víctor

    2011-07-01

    A smart fully automated system is proposed for determination of thorium and uranium in a wide concentration range, reaching environmental levels. The hyphenation of lab-on-valve (LOV) and multisyringe flow injection analysis (MSFIA), coupled to a long path length liquid waveguide capillary cell, allows the spectrophotometric determination of thorium and uranium in different types of environmental sample matrices achieving high selectivity and sensitivity levels. Online separation and preconcentration of thorium and uranium is carried out by means of Uranium and TEtraValents Actinides resin. The potential of the LOV-MSFIA makes possible the full automation of the system by the in-line regeneration of the column and its combination with a smart methodology is a step forward in automation. After elution, thorium(IV) and uranium(VI) are spectrophotometrically detected after reaction with arsenazo-III. We propose a rapid, inexpensive, and fully automated method to determine thorium(IV) and uranium(VI) in a wide concentration range (0-1,200 and 0-2,000 μg L(-1) Th and U, respectively). Limits of detection reached are 5.9 ηg L(-1) of uranium and 60 ηg L(-1) of thorium. Different water sample matrices (seawater, well water, freshwater, tap water, and mineral water), and a channel sediment reference material which contained thorium and uranium were satisfactorily analyzed with the proposed method.

  10. 毛细管电泳-原子光(质)谱联用技术在金属形态与生物分子相互作用研究中的应用%Novel Hyphenated Techniques of Atomic Spectrometry for Metal Species Interaction with Biomolecules

    Institute of Scientific and Technical Information of China (English)

    李妍; 严秀平

    2015-01-01

    Trace metals may be adopted by biological systems to assist in the syntheses and metabolic functions of genes (DNA and RNA)and proteins in the environment.These metals may be beneficial or may pose a risk to humans and other life forms. Novel hybrid techniques are required for studies on the interaction between different metal species and biomolecules,which is significant for biology,biochemistry,nutrition,agriculture,medicine,pharmacy,and environmental science.In recent years, our group dwells on new hyphenated techniques based on capillary electrophoresis (CE),electrothermal atomic absorption spec-trometry (ETAAS),and inductively coupled plasma mass spectroscopy (ICP-MS),and their application for different metal spe-cies interaction with biomolecules such as DNA,HSA,and GSH.The CE-ETAAS assay and CE-ICP-MS assay allow sensitive-ly probing the level of biomolecules such as DNA damage by different metal species and extracting the kinetic and thermodynamic information on the interactions of different metal species with biomolecules,provides direct evidences for the formation of differ-entmetal species-biomolecule adducts.In addition,the consequent structural information were extracted from circular dichroism (CD)and X-ray photoelectron spectroscopy (XPS),Raman spectroscopy,and Fourier transform infrared (FTIR)spectroscopy. The present works represent the most complete and extensive study to date on the interactions between different metal species with biomolecules,and also provide new evidences for and insights into the interactions of different metal species with biomole-cules for further understanding of the toxicological effects of metal species.%金属形态与生物分子相互作用研究对于揭示金属元素在正常生命过程、重大疾病的发生、诊断和治疗过程中的作用机理具有重要意义,发展研究金属元素形态与生物活性分子相互作用的新技术和新方法非常重要。简要总结了十余年来,在发展毛

  11. Pressurised Fluid Extraction of Bioactive Species in Tree Barks : Analysis using Hyphenated Electrochemical Mass Spectrometric Detection

    OpenAIRE

    Co, Michelle

    2010-01-01

    Analytical chemistry has developed throughout time to meet current needs. At present, the interest in biorefinery is growing, due to environmental awareness and the depletion of fossil resources. Biomass from agricultural and forestry industries has proven to be excellent raw material for different processes. Biorefinering valuable species such as bioactive species from biomass, without compromising the primary process of the biomass is highly desirable. Pressurised fluid extraction (PFE) usi...

  12. Affixial Words with Hyphens%需带连字符的词缀词

    Institute of Scientific and Technical Information of China (English)

    陈春勇

    2009-01-01

    词缀词一般无需使用连字符,但亦有少数例外.本文针对名词、动词和形容词前添加前缀时须使用连字符的几种情形进行了探讨,并附带提及了个别词的后缀前也应使用连字符的问题.

  13. Pharmacokinetic study of inosiplex tablets in healthy Chinese volunteers by hyphenated HPLC and tandem MS techniques

    Institute of Scientific and Technical Information of China (English)

    Mo Chen; Yuan Zhang; Xiao-Ting Que; Ya Ding; Lin Yang; Ai-Dong Wen; Tai-Jun Hang

    2013-01-01

    Inosiplex is a compound formulation composed of inosine and p-acetaminobenzoic acid (PABA) salt of N,N-dimethylamino-2-propanol (DIP). This study was to investigate the clinical plasma pharmacokinetic properties of DIP and PABA after single and multiple oral doses of inosiplex tablets in healthy Chinese volunteers. The established LC/MS/MS method for plasma DIP determination had a linear range of 0.02-10 mg/mL, and the HPLC method for plasma PABA determination had a linear range of 0.05-40 mg/mL. Linear pharmacokinetic characteristics were found with single oral doses of 0.5, 1.0 and 2.0 g. No obvious accumulation effects were observed for DIP and PABA.

  14. Hybrid Spaces and Hyphenated Musicians: Secondary Students' Musical Engagement in a Songwriting and Technology Course

    Science.gov (United States)

    Tobias, Evan S.

    2012-01-01

    This case study investigates how secondary students (three individuals and three groups) engaged with music and acted as musicians in a Songwriting and Technology Class (STC), a course involving the creation, performance, recording and production of original music with instruments and music technology. The following research question guided the…

  15. NMR-based metabolomics and hyphenated NMR techniques – a perfect match in natural products research

    DEFF Research Database (Denmark)

    Vinther, Joachim Møllesøe; Wubshet, Sileshi Gizachew; Stærk, Dan

    2015-01-01

    Ethnopharmacology is one of the world’s fastest-growing scientific disciplines encompassing a diverse range of subjects. It links natural sciences research on medicinal, aromatic and toxic plants with socio-cultural studies and has often been associated with the development of new drugs....... The Editors of Ethnopharmacology have assembled an international team of renowned contributors to provide a critical synthesis of the substantial body of new knowledge and evidence on the subject that has emerged over the past decade. Divided into three parts, the book begins with an overview of the subject...... therapeutics across a range of conditions including CNS disorders, cancer, bone and joint health and parasitic diseases. The final part is devoted to regional perspectives covering all continents, providing a state-of-the –art assessment of the status of ethnopharmacological research globally....

  16. Application of Hyphenated Techniques in Speciation Analysis of Arsenic, Antimony, and Thallium

    OpenAIRE

    Rajmund Michalski; Sebastian Szopa; Magdalena Jabłońska; Aleksandra Łyko

    2012-01-01

    Due to the fact that metals and metalloids have a strong impact on the environment, the methods of their determination and speciation have received special attention in recent years. Arsenic, antimony, and thallium are important examples of such toxic elements. Their speciation is especially important in the environmental and biomedical fields because of their toxicity, bioavailability, and reactivity. Recently, speciation analytics has been playing a unique role in the studies of biogeochemi...

  17. Dropping the Hyphen? Becoming Latino(a)-American through Racialized Assimilation

    Science.gov (United States)

    Golash-Boza, Tanya

    2006-01-01

    Early assimilation theorists predicted the eventual loss of ethnic distinctiveness for immigrants in the United States. In this paper, the author not only questions the possibilities that Latino and Latina Americans have for losing their ethnic distinctiveness, but also proposes that these possibilities vary widely within the Hispanic population.…

  18. Gas chromatography/ion mobility spectrometry as a hyphenated technique for improved explosives detection and analysis

    Science.gov (United States)

    Mercado, AL; Marsden, Paul

    1995-01-01

    Ion Mobility Spectrometry (IMS) is currently being successfully applied to the problem of on-line trace detection of plastic and other explosives in airports and other facilities. The methods of sample retrieval primarily consist of batch sampling for particulate residue on a filter card for introduction into the IMS. The sample is desorbed into the IMS using air as the carrier and negative ions of the explosives are detected, some as an adduct with a reagent ion such as Cl(-). Based on studies and tests conducted by different airport authorities, this method seems to work well for low vapor pressure explosives such as RDX and PETN, as well as TNT that are highly adsorptive and can be found in nanogram quantities on contaminated surfaces. Recently, the changing terrorist threat and the adoption of new marking agents for plastic explosives has meant that the sample introduction and analysis capabilities of the IMS must be enhanced in order to keep up with other detector developments. The IMS has sufficient analytical resolution for a few threat compounds but the IMS Plasmogram becomes increasingly more difficult to interpret when the sample mixture gets more complex.

  19. Development of multidimensional liquid chromatographic methods hyphenated to mass spectrometry, preparation and analysis of complex biological samples

    OpenAIRE

    Delmotte, Nathanaël

    2007-01-01

    Immunoadsorbers based on monolithic epoxy-activated CIM disks have been developed in order to target biomarkers of heart diseases. The developed immunoadsorbers permitted to selectively isolate myoglobin and NT-proBNP from human serum. Anti-NT-proBNP-CIM disks permitted a quantitative isolation of NT-proBNP at concentrations down to 750 amol/µL in serum (R2 = 0.998). Six different restricted access materials have been evaluated with respect to their ability to remove hemoglobin from hemoly...

  20. Sustainability Study on Heavy Metal Uptake in Neem Biodiesel Using Selective Catalytic Preparation and Hyphenated Mass Spectrometry

    OpenAIRE

    Mirella Elkadi; Avin Pillay; Johnson Manuel; Mohammad Zubair Khan; Sasi Stephen; Arman Molki

    2014-01-01

    It is common knowledge that the presence of trace metals in biofuels can be detrimental to the environment and long-term sustainable development. This study provides an insight into selective catalytic preparation of biofuel to compare uptake of trace metals in the biodiesel fraction with preferential base catalysts. The role of specific metal hydroxides in controlling trace metal content in biofuel production is relatively unexplored, and the effect of different homogeneous catalysts (NaOH, ...

  1. Four new degradation products of doxorubicin:An application of forced degradation study and hyphenated chromatographic techniques

    Institute of Scientific and Technical Information of China (English)

    Dheeraj Kaushik; Gulshan Bansal

    2015-01-01

    Forced degradation study on doxorubicin (DOX) was carried out under hydrolytic condition in acidic, alkaline and neutral media at varied temperatures, as well as under peroxide, thermal and photolytic conditions in accordance with International Conference on Harmonization (ICH) guidelines Q1(R2). It was found extremely unstable to alkaline hydrolysis even at room temperature, unstable to acid hy-drolysis at 80 °C, and to oxidation at room temperature. It degraded to four products (O-I-O-IV) in oxidative condition, and to single product (A-I) in acid hydrolytic condition. These products were re-solved on a C8 (150 mm × 4.6 mm, 5μm) column with isocratic elution using mobile phase consisting of HCOONH4 (10 mM, pH 2.5), acetonitrile and methanol (65:15:20, / / ). Liquid chromatography-pho-todiode array (LC-PDA) technique was used to ascertain the purity of the products noted in LC-UV chromatogram. For their characterization, a six stage mass fragmentation (MS6) pattern of DOX was outlined through mass spectral studies in positive mode of electrospray ionization (+ESI) as well as through accurate mass spectral data of DOX and the products generated through liquid chromato-graphy-time of flight mass spectrometry (LC-MS-TOF) on degraded drug solutions. Based on it, O-I-O-IV were characterized as 3-hydroxy-9-desacetyldoxorubicin-9-hydroperoxide, 1-hydroxy-9-desacetyldox-orubicin-9-hydroperoxide, 9-desacetyldoxorubicin-9-hydroperoxide and 9-desacetyldoxorubicin, re-spectively, whereas A-I was characterized as deglucosaminyl doxorubicin. While A-I was found to be a pharmacopoeial impurity, all oxidative products were found to be new degradation impurities. The mechanisms and pathways of degradation of doxorubicin were outlined and discussed.

  2. Putting Ourselves on the Line: The Epistemology of the Hyphen, Intersubjectivity and Social Responsibility in Qualitative Research

    Science.gov (United States)

    Granek, Leeat

    2013-01-01

    As researchers, we are intertwined in our research relationships in two ways that put us on the line. First, our very beings are co-constituted and developed in an intersubjective exchange with the people we work with. Acknowledging our interdependence frees us to take an empathetic and hermeneutic stance that I have termed the "epistemology…

  3. The Hyphen of National Culture : The Paradox of National Distinctiveness in Belgium and the Netherlands, 1860-1918

    NARCIS (Netherlands)

    Tollebeek, Jo

    2010-01-01

    At the turn of the 20th century, intellectuals and artists in Belgium and the Netherlands were keen to define their respective national identities. One of the most striking ways of doing this was based on a paradox: in both Belgium and the Netherlands the idea came into being that their national dis

  4. 连字号复合词的语体分析%Genre Analysis of Hyphenated Compounds

    Institute of Scientific and Technical Information of China (English)

    赵琼

    2009-01-01

    在英语构词法中,复合词占有较大比例.根据拼写规则,复合词可以分为三类: 固定复合词、连字号复合词和开放型复合词.连字号复合词更以形象生动、变化无穷和经济简洁的表现手法著称.文章从语体分析入手,研究连字号复合词的语体色彩、特征和功能.

  5. 分析仪器联用技术的发展动向%Development of Instrument Hyphenated Technology

    Institute of Scientific and Technical Information of China (English)

    赵宏

    2006-01-01

    分析仪器联用技术已在环境样品分析中得到应用,并有广阔的发展前景.本文介绍了色谱-色谱、色谱-原子光谱、离子色谱联用技术、色谱-质谱、色谱-傅立叶变换红外光谱、色谱-核磁共振波谱(NMR)联用技术在分析环境样品方面的应用.

  6. Word Formation with Hyphen and Related Translation%连字符构词探索及其翻译

    Institute of Scientific and Technical Information of China (English)

    李砚霞

    2009-01-01

    连字符构词因其同其他构词之间的特殊联系以及它自身构成的灵活性、广泛性的特点,它的构词规律应该被视为独立的构词法去探索;翻译连字符构词应在掌握其他构词翻译方法和技巧的基础上更加关注连字符构词语义整体性、单一性、简洁性的特点.

  7. Rapid Identification of Bibenzyls of Stemona sessilifolia using Hyphenated LC-UV-NMR and LC-MS Methods

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    As a part of the ongoing search for new constituents of Stemona species in China, chemical investigation of Stemona sessilifolia, a plant used in the traditional Chinese medicine to treat respiratory disorders, was carried out. To identify the chemical components rapidly, a selected sample of S. sessilifolia containing bibenzyls was tested using LC-ESIMS and analyzed further using stop-flow LC-UV-NMR, which was sensitive for the detection of the main constituents. LC microfractions were collected using the LC-UV-NMR technique and HR-EIMS off-line analysis was carried out on the collected fractions. This chemical screening strategy allowed for the on-line identification of the main constituents of S. sessilifolia and provided information that was useful for a further peak-guided isolation procedure.Using these methods, four bibenzyls were isolated: two known compounds, 3,5-dihydroxy-4-methyl bibenzyl(1) and 3,5-dihydroxy-2'-methoxy-4-methyl bibenzyl ( 2 ), and two novel compounds, 3, 3'-dihydroxy-5, 6'-dimethoxy bibenzyl (3) and 3,5-dihydroxy-2' ,5'-dimethoxy bibenzyl (4).

  8. Dual-Stage Consumable-Free Thermal Modulator for the Hyphenation of Thermal Analysis, Gas Chromatography, and Mass Spectrometry.

    Science.gov (United States)

    Wohlfahrt, Sebastian; Fischer, Michael; Varga, Janos; Saraji-Bozorgzad, Mohammad-Reza; Matuschek, Georg; Denner, Thomas; Zimmermann, Ralf

    2016-01-01

    The design of the so-called "Peltier modulator" is presented. It is a new dual-stage consumable-free thermal modulator for thermal analysis-gas chromatography-mass spectrometry (TA-GC-MS). It requires only electrical power for operation as it facilitates thermo-electric coolers instead of cryogenics for trapping and resistive on-column heating for reinjection. Trapping and desorption temperatures as well as modulation cycles are freely adjustable. The stationary phase for the trapping region can be selected to suit the specific application, since common fused silica capillary is used. The Peltier modulator's performance is demonstrated with a broad range of different standard substances and with heavy crude oil as a complex real life sample. Successful modulation from n-pentane to pyrene (boiling points = 36/394 °C) is presented. The produced peaks show the narrowest bandwidths ever reported for a consumable-free thermal modulator, i.e., 12.8 ± 1.2 ms for n-pentadecane. The Peltier modulator is rugged, cost-effective, requires low maintenance, and decreases security issues significantly, compared to commercial available solutions using liquid N2/CO2. PMID:26606252

  9. Speciation of gadolinium in surface water samples and plants by hydrophilic interaction chromatography hyphenated with inductively coupled plasma mass spectrometry.

    Science.gov (United States)

    Lindner, Uwe; Lingott, Jana; Richter, Silke; Jakubowski, Norbert; Panne, Ulrich

    2013-02-01

    Hydrophilic interaction chromatography (HILIC) coupled with inductively coupled plasma mass spectrometry (ICP-MS) was optimized for speciation analysis of gadolinium-based contrast agents in environmental samples, in particular surface river waters and plants. Surface water samples from the Teltow channel, near Berlin, were investigated over a distance of 5 km downstream from the influx of a wastewater treatment plant. The total concentration of gadolinium increased significantly from 50 to 990 ng L(-1) due to the influx of the contrast agents. After complete mixing with the river water, the concentration remained constant over a distance of at least 4 km. Two main substances [Dotarem(®) (Gd-DOTA) and Gadovist(®) (Gd-BT-DO3A)] have been identified in the river water using standards. A gadolinium-based contrast agent, possibly Gd-DOTA (Dotarem(®)), was also detected in water plant samples taken from the Teltow channel. Therefore, uptake of contrast agents [Gadovist(®) (Gd-BTDO3A), Magnevist(®) (Gd-DTPA), Omniscan(®) (Gd-DTPA-BMA), Dotarem(®) (Gd-DOTA), and Multihance(®) (Gd-BOPTA)] by plants was investigated in a model experiment using Lepidium sativum (cress plants). HILIC-ICP-MS was used for identification of different contrast agents, and a first approach for quantification using aqueous standard solutions was tested. For speciation analysis, all investigated contrast agents could be extracted from the plant tissues with a recovery of about 54 % for Multihance(®) (Gd-BOPTA) up to 106 % for Gadovist(®) (Gd-BT-DO3A). These experiments demonstrate that all contrast agents investigated are transported from the roots to the leaves where the highest content was measured.

  10. Hyphenated chromatographic techniques for the rapid screening and identification of antioxidants in methanolic extracts of pharmaceutically used plants .

    NARCIS (Netherlands)

    Exarchou, V.; Fiamegos, Y.C.; Beek, van T.A.; Nanos, C.G.; Vervoort, J.J.M.

    2006-01-01

    Phytochemical analysis is an important scientific research area, which normally relies on a number of rather laborious and time-consuming techniques for compound identification. Isolation of the ingredients of plant extracts in adequate quantities for spectral and biological analysis was the basis o

  11. A New Hyphenated μ Trap—GC—Surface Acoustic Wave (SAW) Based Electronic Nose For Monitoring Of Coffee Quality

    Science.gov (United States)

    Carvalho, Mauro; Voigt, Achim; Rapp, Michael

    2009-05-01

    An easy-to-use and versatile analytical method for complex matrix analisis like coffee was developed. The system consists of a microtrap sample preparation, a home made simplified gaschomatographic separation unit and an 8-fold surface acoustic wave based sensors (SAW) array detector. For the coffee quality analysis a successful discrimination of three coffee samples could be achieved. The system would be further developed into a fully automated, low cost version that can be broadly used by the coffee producers.

  12. A broad-based study on hyphenating new ionization technologies with MS/MS for PTMs and tissue characterization.

    Science.gov (United States)

    Marshall, Darrell D; Inutan, Ellen D; Wang, Beixi; Liu, Chih-Wei; Thawoos, Shameemah; Wager-Miller, James; Mackie, Ken; Trimpin, Sarah

    2016-06-01

    Matrix-assisted ionization (MAI) is a newly discovered method for converting compounds from the solid phase to gas-phase ions having charge states similar to electrospray ionization (ESI), but without the need for high-energy sources such as lasers or high voltage. Laserspray ionization (LSI) is a subset of MAI that uses a laser to provide high spatial resolution analyses, but the laser is not directly involved in the ionization process. These methods produce multiply-charged analyte ions that are useful for characterizing compounds directly from surfaces using advanced characterization technologies. Because the multiply-charged ions originate from charged matrix clusters, efficient desolvation of the matrix is a prerequisite. Here, we report on the utility of collision-induced dissociation (CID) and electron transfer dissociation (ETD) coupled to mass spectrometry using several MAI and LSI matrices for peptide and protein characterization employing mass spectrometers from two manufacturers. The information obtained is similar to that using ESI for most analyses and superior to matrix-assisted laser desorption/ionization (MALDI) as is shown for intact proteins and protein digests directly from mouse brain tissue sections. The ionization processes are soft so that posttranslational modification (e.g. phosphorylation) sites are readily determined. Instances where ETD or CID in conjunction with MAI failed are attributed to lack of desolvation of charged matrix:analyte particles. PMID:27093917

  13. On-line sample-pre-treatment schemes for trace-level determinations of metals by coupling flow injection or sequential injection with ICP-MS

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2003-01-01

    Within the last decade, the first generation of flow injection (FI) has been supplemented by sequential injection (SI), also termed the second generation, and, recently, by the third generation, i.e., SI-Lab-on-Valve (SI-LOV). As apparent from the literature, FI and/or SI have become dominant...

  14. Trends and perspectives of flow injection/sequential injection on-line sample-pretreatment schemes coupled to ETAAS

    DEFF Research Database (Denmark)

    Wang, Jianhua; Hansen, Elo Harald

    2005-01-01

    Flow injection (FI) analysis, the first generation of this technique, became in the 1990s supplemented by its second generation, sequential injection (SI), and most recently by the third generation (i.e.,Lab-on-Valve). The dominant role played by FI in automatic, on-line, sample pretreatments...

  15. Tre generationer af Flow Injection Analysis

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Chomchoei, Roongrat; Long, Xiangbao

    2004-01-01

    Siden introduktionen af FIA har en række videreudviklinger resulteret i Sequential Injection Analysis (SIA) og senest i Lab-on-Valve (LOV)-metodikken. Her beskrives disse, og der gives eksempler på, hvordan metoderne kan bruges til at bestemme sporstofkoncentrationer af metaller i komplekse...

  16. How Flow Injection Analysis (FIA) over the past 25 years has changed our way of performing chemical analyses

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Miró, Manuel

    2007-01-01

    Briefly looking back on the impact of flow injection analysis (FIA), as reflected in the rapid growth of publications in the scientific literature, and touching upon many of the novel and unique analytical chemical possibilities that FIA and its sequels, sequential injection analysis (SIA) and Lab-on-Valve...

  17. Gas-phase separation of drugs and metabolites using modifier-assisted differential ion mobility spectrometry hyphenated to liquid extraction surface analysis and mass spectrometry.

    Science.gov (United States)

    Porta, Tiffany; Varesio, Emmanuel; Hopfgartner, Gérard

    2013-12-17

    The present work describes an alternative generic approach to LC-MS for the analysis of drugs of abuse as well as their metabolites in post-mortem tissue samples. The platform integrates liquid extraction surface analysis (LESA) for analytes tissue extraction followed by differential ion mobility spectrometry (DMS) mass spectrometry for analytes gas phase separation. Detection is performed on a triple quadrupole linear ion trap using the selected reaction monitoring mode for quantification as well as product ion scan mode for structural confirmatory analyses. The major advantages of the platform are that neither chromatographic separation nor extensive sample preparation are required. In DMS the combination of a high separation voltage (i.e., up to 4 kV) together with organic modifiers (e.g., alcohols, acetonitrile, acetone) added in the drift gas is required to achieve the separation of isomeric metabolites, such as the ones of cocaine and tramadol. DMS also separates morphine from its glucuronide metabolites, which allows for preventing the overestimation of morphine in case of fragmentation of the glucuronides in the atmospheric-to-vacuum interface of the mass spectrometer. Cocaine, opiates, opioids, amphetamines, benzodiazepines and several of their metabolites could be identified in post-mortem human kidney and muscle tissue based on simultaneous screening and confirmatory analysis in data-dependent acquisition mode using an analyte-dependent compensation voltage to selectively transmit ions through the DMS cell to the mass analyzer. Quantitative performance of the LESA-DMS-MS platform was evaluated for cocaine and two of its metabolites spotted onto a tissue section using deuterated internal standard. Analyte's responses were linear from 2 to 1000 pg on tissue corresponding to a limit of detection in the order of nanograms of analyte per gram of tissue. Accuracy and precision based on QC sample was found to be less than 10%. Replicate analyses of cocaine and its metabolites in forensic samples showed an intra- and inter-sections variability of less than 25%. PMID:24251629

  18. Towards early detection of the hydrolytic degradation of poly(bisphenol A)carbonate by hyphenated liquid chromatography and comprehensive two-dimensional liquid chromatography

    NARCIS (Netherlands)

    Coulier, L.; Kaal, E.R.; Hankemeier, Th.

    2006-01-01

    The hydrolytic degradation of poly(bisphenol A)carbonate (PC) has been characterized by various liquid chromatography techniques. Size exclusion chromatography (SEC) showed a significant decrease in molecular mass as a result of hydrolytic degradation, while 'liquid chromatography at critical condit

  19. Development of a triple hyphenated HPLC-radical scavenging detection-DAD-SPE-NMR system for the rapid identification of antioxidants in complex plant extracts

    NARCIS (Netherlands)

    Pukalskas, A.; Beek, van T.A.; Waard, de P.

    2005-01-01

    A rapid method for the simultaneous detection and identification of radical scavenging compounds in plant extracts was developed by combining an HPLC with on-line radical scavenging using DPPH as a model radical and an HPLC¿DAD¿SPE¿NMR system. Using this method a commercial rosemary extract was inve

  20. New on-line separation workflow of microbial metabolites via hyphenation of analytical and preparative comprehensive two-dimensional liquid chromatography.

    Science.gov (United States)

    Yan, Xia; Wang, Li-Juan; Wu, Zhen; Wu, Yun-Long; Liu, Xiu-Xiu; Chang, Fang-Rong; Fang, Mei-Juan; Qiu, Ying-Kun

    2016-10-15

    Microbial metabolites represent an important source of bioactive natural products, but always exhibit diverse of chemical structures or complicated chemical composition with low active ingredients content. Traditional separation methods rely mainly on off-line combination of open-column chromatography and preparative high performance liquid chromatography (HPLC). However, the multi-step and prolonged separation procedure might lead to exposure to oxygen and structural transformation of metabolites. In the present work, a new two-dimensional separation workflow for fast isolation and analysis of microbial metabolites from Chaetomium globosum SNSHI-5, a cytotoxic fungus derived from extreme environment. The advantage of this analytical comprehensive two-dimensional liquid chromatography (2D-LC) lies on its ability to analyze the composition of the metabolites, and to optimize the separation conditions for the preparative 2D-LC. Furthermore, gram scale preparative 2D-LC separation of the crude fungus extract could be performed on a medium-pressure liquid chromatograph×preparative high-performance liquid chromatography system, under the optimized condition. Interestingly, 12 cytochalasan derivatives, including two new compounds named cytoglobosin Ab (3) and isochaetoglobosin Db (8), were successfully obtained with high purity in a short period of time. The structures of the isolated metabolites were comprehensively characterized by HR ESI-MS and NMR. To be highlighted, this is the first report on the combination of analytical and preparative 2D-LC for the separation of microbial metabolites. The new workflow exhibited apparent advantages in separation efficiency and sample treatment capacity compared with conventional methods. PMID:27517521

  1. Characterizing Environmental Transformation of Multi-walled Carbon Nanotubes and Carbon Nano-Fiber Composites using Thermal Analysis and Related Hyphenated Techniques

    Science.gov (United States)

    Thermogravimetric analysis (TGA) coupled with gas chromatography and mass spectroscopy (TGA/GCMS), for the evolved gas analysis, has given insight to the stability and kinetics of structural changes and determining adsorbed organics to nanomaterials and nanocomposites. TGA is als...

  2. 核磁共振联用技术在代谢物结构研究中的应用%Application of NMR hyphenation for identification metabolites

    Institute of Scientific and Technical Information of China (English)

    胡增峰; 黄荣清; 肖炳坤; 杨建云

    2008-01-01

    核磁共振联用技术是体内药物代谢产物结构鉴定的强大工具.本文综述固相萃取-核磁共振、液相色谱-核磁共振、液相色谱-核磁共振-质谱等联用技术在研究生物样品中代谢物结构的应用.

  3. 出版物中英语单词移行的技术性细节%Conventional Uses of End-of-Line Hyphenation in Publishing

    Institute of Scientific and Technical Information of China (English)

    王伟

    2014-01-01

    为促使出版物中英语单词的移行规范,按照相关细则,结合示例,归纳了单音节词、专有名词、缩写词、首字母缩略词、缩约词、数字及易产生误解词等不可移行词语;解释了多音节词、带连字符词、带双写辅音字母词、带有前后缀词等可移行词语;提及了行末和行首、网址与电子邮箱、连续移行与隔页移行等应注意的环节.

  4. 英文论文写作中如何正确使用连字符%On Correct Use of Hyphens in Writing English Papers

    Institute of Scientific and Technical Information of China (English)

    宋双明

    2004-01-01

    英文科技论文的特点之一是术语较多,因此经常会遇到连字符的使用问题.本文对正确使用连字符进行了归纳、总结、整理,以期规范使用语言,提高科技论文英文写作与编辑水平.

  5. Hyphenated chromatographic analysis of bioactive gallic acid and quercetin in Hygrophila auriculata (K. Schum) Heine growing wildly in marshy places in India by validated HPTLC method

    Institute of Scientific and Technical Information of China (English)

    Md Sarfaraj Hussain; Sheeba Fareed; Mohammad Ali

    2012-01-01

    Objective: A simple, accurate, and rapid high-performance thin-layer chromatographic (HPTLC) method for simultaneous quantification of the two biologically active flavonoidal compounds, gallic acid and quercetin, in Hygrophila auriculata (K. Schum) Heine (HA) has been established and validated. Methods: Chromatography was performed on aluminium foil-backed silica gel 60 F254 HPTLC plates with the binary mobile phase toluene: ethyl acetate: formic acid (5:4:1, v/v/v). Ultraviolet detection was performed densitometrically at the maximum absorbance wavelength, 270nm. The method was validated for precision, recovery, robustness, specificity, and detection and quantification limits, in accordance with ICH guidelines. Results: The system was found to give compact spots for gallic acid (GA) and quercetin (QE) (Rf value of 0.31 and 0.50, respectively). The limit of detection (23 and 41 ng band-1) limit of quantification (69 and 123 ng band-1), recovery (99.4-99.9 and 98.7-99.4%), and precision (i.e ≤1.98 and 1.97) were satisfactory for gallic acid and quercetin respectively. Linearity range for GA and QE were 100-1000 (r 2= 0.9991) and 150-900 ng band-1 (r2= 0.9956) and the contents estimated as 0.28±0.01% and 0.41±0.01% w/w respectively.Conclusions:This simple, precise and accurate method gave good resolution from other constituents present in the extract. The method has been successfully applied in the analysis and routine quality control of herbal material and formulations containing Hygrophila auriculata (K. Schum) Heine.

  6. Dynamic Precoatings for Hyphenated CE Applications%动态预涂层在CE联用技术中的应用

    Institute of Scientific and Technical Information of China (English)

    William W.P.Chang; Christine Hobson; David C.Bomberger; Luke V.Schneider

    2007-01-01

    毛细管电泳与传统分离方法相比,具有分析时间短、分辨率高、样品/缓冲液用量少、易于自动化、功能多样性等优点.尽管如此,毛细管电泳在分析领域仍未能展现出全部的潜力.这是由于在大多数要求比较苛刻的实际应用中,毛细管电泳难以获得较高的重现性.本文对该问题进行了阐述,并提出了一个很有前途的解决方法.

  7. 论英语连合词的形态语义特征%Morphological and semantic features of hyphenated English compounds

    Institute of Scientific and Technical Information of China (English)

    徐宏亮

    2012-01-01

    复合法是英语新词的重要构词手段,是现代英语的一大特征.分析2647个带连字符的英语复合词(连合词),揭示它们的构词形态模式及语义特征,并指出连合词的有效使用是较高语言能力的一个重要标志.

  8. Simultaneous determination of benzene and phenol in heat transfer fluid by head-space gas chromatography hyphenated with ion mobility spectrometry.

    Science.gov (United States)

    Criado-García, L; Garrido-Delgado, R; Arce, L; López, F; Peón, R; Valcárcel, M

    2015-11-01

    The quantitative determination of some compounds such as benzene and phenol in a complex matrix by ion mobility spectrometry (IMS) can be a difficult task, due to the influence of other components present in the matrix and the chemical properties of both compounds, such as their high volatility and low proton affinity. Monitoring of these compounds in a heat transfer fluid (HTF) is essential to check the correct working of a thermosolar plant and for safety and environmental reasons. Benzene and phenol, among other compounds, are produced when HTF is exposed to high temperatures in continuous cycles and their presence can decrease the efficiency of HTF. For the first time, a headspace module coupled to a gas chromatography column in combination with an IMS (with a tritium ionization source) has been optimized and fully validated to simultaneously quantify benzene and phenol in HTF. The limit of detection (LOD) and limit of quantification (LOQ) achieved with the method proposed were 0.011 and 0.038 g L(-1) and 0.004 and 0.014 g L(-1) for benzene and phenol respectively. The precision of the method was evaluated in terms of repeatability and reproducibility with all values lower than 9.2% and 13.3%, respectively. Results demonstrated that benzene and phenol were generated in the HTF heating process, and its concentration increased with heating time (approximately 483 h). The average concentration values for benzene and phenol in degraded HTF samples were not significantly different to values obtained using a gas chromatography-flame ionization detector instrument. Therefore, IMS is a promising technique for in-field quality control of HTF in a thermosolar plant due to its speed, versatility, sensitivity and selectivity to quantify these degradation compounds. PMID:26452912

  9. ARSENIC SPECIATION IN CHINESE SEAFOODS BY USING HYPHENATED TECHNIQUES%采用联用技术测定中国海产品中砷的形态

    Institute of Scientific and Technical Information of China (English)

    韦超; 李卫华; 张超; 张新荣; VANHULLEMarijn,CO; CORNELISRita

    2003-01-01

    A study was carried out to determine arsenic species in seafood samples collected from Chinese sea. The information about arsenic species in samples was provided by high performance liquid chromatography-inductively coupled plasma-mass spectrometer (HPLC-ICP-MS) and electrospray tandem mass spectrometry (ES-MS-MS). The arsenic species in thirty Chinese edible seafoods, including algae, fish, crab, shrimp, mussels, oysters, and clams popularly ingested by Chinese people as regular foods, were examined in the present report. Arsenosugars were detected in all of the extracted algae samples (1.5-33.8μg*g-1 dry weight) and some shellfish samples (0.018-0.78μg*g-1 wet weight). Arsenobetaine was detected in all of the extracted fish and shellfish samples (0.025-6.604μg*g-1 wet weight). In contrast, inorganic arsenic was only present in the examined fish and shellfish samples, at levels less than 2% of the total arsenic. The study provides information about a possible distribution pattern of arsenic species in seafood products.

  10. Antioxidant Properties and Hyphenated HPLC-PDA-MS Profiling of Chilean Pica Mango Fruits (Mangifera indica L. Cv. piqueño

    Directory of Open Access Journals (Sweden)

    Javier E. Ramirez

    2013-12-01

    Full Text Available Antioxidant capacities and polyphenolic contents of two mango cultivars from northern Chile, one of them endemic of an oasis in the Atacama Desert, were compared for the first time. Twenty one phenolic compounds were detected in peel and pulp of mango fruits varieties Pica and Tommy Atkins by HPLC-PDA-MS and tentatively characterized. Eighteen compounds were present in Pica pulp (ppu, 13 in Pica peel (ppe 11 in Tommy Atkins pulp (tpu and 12 in Tommy Atkins peel (tpe. Three procyanidin dimers (peaks 6, 9 and 10, seven acid derivatives (peaks 1–4, 11, 20 and 21 and four xanthones were identified, mainly mangiferin (peak 12 and mangiferin gallate, (peak 7, which were present in both peel and pulp of the two studied species from northern Chile. Homomangiferin (peak 13 was also present in both fruit pulps and dimethylmangiferin (peak 14 was present only in Tommy pulp. Pica fruits showed better antioxidant capacities and higher polyphenolic content (73.76/32.23 µg/mL in the DPPH assay and 32.49/72.01 mg GAE/100 g fresh material in the TPC assay, for edible pulp and peel, respectively than Tommy Atkins fruits (127.22/46.39 µg/mL in the DPPH assay and 25.03/72.01 mg GAE/100 g fresh material in the TPC assay for pulp and peel, respectively. The peel of Pica mangoes showed also the highest content of phenolics (66.02 mg/100 g FW measured by HPLC-PDA. The HPLC generated fingerprint can be used to authenticate Pica mango fruits and Pica mango food products.

  11. Simultaneous determination of benzene and phenol in heat transfer fluid by head-space gas chromatography hyphenated with ion mobility spectrometry.

    Science.gov (United States)

    Criado-García, L; Garrido-Delgado, R; Arce, L; López, F; Peón, R; Valcárcel, M

    2015-11-01

    The quantitative determination of some compounds such as benzene and phenol in a complex matrix by ion mobility spectrometry (IMS) can be a difficult task, due to the influence of other components present in the matrix and the chemical properties of both compounds, such as their high volatility and low proton affinity. Monitoring of these compounds in a heat transfer fluid (HTF) is essential to check the correct working of a thermosolar plant and for safety and environmental reasons. Benzene and phenol, among other compounds, are produced when HTF is exposed to high temperatures in continuous cycles and their presence can decrease the efficiency of HTF. For the first time, a headspace module coupled to a gas chromatography column in combination with an IMS (with a tritium ionization source) has been optimized and fully validated to simultaneously quantify benzene and phenol in HTF. The limit of detection (LOD) and limit of quantification (LOQ) achieved with the method proposed were 0.011 and 0.038 g L(-1) and 0.004 and 0.014 g L(-1) for benzene and phenol respectively. The precision of the method was evaluated in terms of repeatability and reproducibility with all values lower than 9.2% and 13.3%, respectively. Results demonstrated that benzene and phenol were generated in the HTF heating process, and its concentration increased with heating time (approximately 483 h). The average concentration values for benzene and phenol in degraded HTF samples were not significantly different to values obtained using a gas chromatography-flame ionization detector instrument. Therefore, IMS is a promising technique for in-field quality control of HTF in a thermosolar plant due to its speed, versatility, sensitivity and selectivity to quantify these degradation compounds.

  12. Precise isotope-ratio determination by CGC hyphenated to ICP-MCMS for speciation of trace amounts of gaseous sulfur, with SF6 as example compound.

    Science.gov (United States)

    Krupp, Eva M; Pécheyran, Christophe; Meffan-Main, Simon; Donard, Olivier F X

    2004-01-01

    Capillary gas chromatography coupled to an inductively coupled plasma mass spectrometer with multiple-collector detection (GC-ICP-MCMS) has been used to assess the precision and instrumental mass bias in sulfur isotope-ratio determination for the gaseous sulfur species SF6. The isotopic composition of the compound was certified by the institute for reference materials and measurements (IRMM, Belgium) and is available as PIGS 2010. Integration of the peaks (peak half-width 1.4 s) was performed using a special peak-integration method based on definition of the integration area by assessment of a uniform isotope-ratio area within the chromatographic peak. Instrumental mass bias was determined to be approximately 12% per mass unit and proved to be stable in the concentration range measured. Replicate injections of 2, 10, 20, and 30 ng (as S) SF6 diluted in argon gave precision for the 32S/34S ratio from 0.6% RSD for 2-ng injections to 0.03% RSD for 30-ng injections. The 32S/33S and 33S/34S isotope-ratio precision was better than 0.4% RSD for injections of 10 ng (as S) and higher. Detection limits were in the absolute pg range for all measured sulfur isotopes. PMID:14618293

  13. Hyphenation of ultra performance liquid chromatography (UPLC) with inductively coupled plasma mass spectrometry (ICP-MS) for fast analysis of bromine containing preservatives

    DEFF Research Database (Denmark)

    Bendahl, Lars; Hansen, Steen Honoré; Gammelgaard, Bente;

    2006-01-01

    Ultra performance liquid chromatography (UPLC) was coupled to inductively coupled plasma mass spectrometry (ICP-MS) for fast analysis of three bromine-containing preservatives, monitoring the 79Br and 81Br isotopes simultaneously. Due to the efficiency of the 1.7 microm column packing material...... analysis of bromine-containing preservatives in commercially available cosmetic products....

  14. Elucidation of flavonoids from Carissa congesta, Polyalthia longifolia, and Benincasa hispida plant extracts by hyphenated technique of liquid chromatography-mass spectroscopy

    Directory of Open Access Journals (Sweden)

    Gaurav M Doshi

    2016-01-01

    Full Text Available Background: Carissa congesta (CC, Polyalthia longifolia (PL, and Benincasa hispida (BH are economically important plants. Objective: Current research encompasses identification of quercetin and rutin and their analogues by liquid chromatography-mass spectroscopy (LC-MS from the selected plant species. Materials and Methods: Fresh roots, leaves, and seeds of CC, PL, and BH plants respectively were shade-dried followed by extraction and elucidation of rutin and quercetin by LC-MS. Results: Structural elucidation of CC, PL, and BH extracts revealed the presence of flavonoids such as quercetin (m/z 301 and rutin (m/z 610 as the parent ions along with presence of close analogues such as quercetin-O-hexoside, Vicenin 2, quercetin-3-O-xyloside/arabinoside, and quercetin-3-O-glucoside were identified as fragments. Conclusions: Thus, CC, PL, and BH extracts revealed the presence of flavonoids belonging to the class of flavonols such as rutin and quercetin.

  15. Introduction

    DEFF Research Database (Denmark)

    Hahonou, Eric Komlavi; Lecocq, Baz

    2015-01-01

    -abolition, and post-emancipation share the hyphen in common. The hyphen in this context connects the past to the present, the work of the historian to the work of the anthropologist, the slave to the master. But the hyphen also indicates a temporal disruption or discontinuity. We must bridge the historical...

  16. Use of flow injection and sequential injection analysis schemes for the determination of trace-level concentrations of metals in complex matrices by ETAAS and ICPMS

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    2005-01-01

    to facilitate the desired sensitivity and selectivity of measurement. Such pretreatment schemes are advantageously performed in flow injection (FI) or sequential injection (SI) manifolds, where all unit operations can be effected on-line and under enclosed and strictly controlled conditions. Various separation...... and characteristics of FI and SI, we present, via selected examples, various separation/preconcentration FI/Sl schemes for the determination of trace levels of metals, with particular emphasis on the use of the novel extension of FI/SI, that is, the so-called lab-on-valve concept....

  17. Implementation of suitable flow injection/sequential-sample separation/preconcentration schemes for determination of trace metal concentrations using detection by electrothermal atomic absorption spectrometry and inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Wang, Jianhua

    2002-01-01

    ) are presented and discussed. Demonstrating that such pretreatments advantageously are to be performed in flow injection (FI) or sequential injection (SI) manifolds, where all appropriate unit operations can be effected under enclosed and strictly controlled conditions, procedures based on ion......-exchange, precipitation/coprecipitation, adsorption, liquid-liquid extraction, extraction/back-extraction and hydride generation are reviewed. Emphasising the use of SI-systems, special attention is paid to the use of the newly introduced approach termed the lab-on-valve (LOV), where all necessary manipulations required...... prior to detection are effected in a microconduit placed on top of an SI selection valve....

  18. Flow Injection Analysis

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    2004-01-01

    This chapter provides an introduction to automated chemical analysis, which essentially can be divided into two groups: batch assays, where the solution is stationary while the container is moved through a number of stations where various unit operations performed; and continuous-flow procedures......, where the system is stationary while the solution moves through a set of conduits in which all required manipulations are performed. Emphasis is placed on flow injection analysis (FIA) and its further developments, that is, sequential injection analysis (SIA) and the Lab-on-Valve (LOV) approach. Since...

  19. Screening for illicit drugs in pooled human urine and urinated soil samples and studies on the stability of urinary excretion products of cocaine, MDMA, and MDEA in wastewater by hyphenated mass spectrometry techniques

    DEFF Research Database (Denmark)

    Mardal, Marie; Kinyua, Juliet; Ramin, Pedram;

    2016-01-01

    were the most frequently detected illicit drugs; an analytical method was developed to quantify their excretion products. Hydroxymethoxymethamphetamine (HMMA), 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyamphetamine (MDA), HMMA sulfate (HMMA-S), benzoylecgonine (BE), and cocaethylene...... (CE) had 85–102% of initial concentration after 8 h of incubation, whereas COC and ecgonine methyl ester (EME) had 74 and 67% after 8 h, respectively. HMMA showed a net increase during 24 h of incubation (107% ± 27, n = 8), possibly due to the cleavage of HMMA conjugates, and biotransformation of MDMA....... The results suggest HMMA as analytical target for MDMA consumption in WBE, due to its stability in wastewater and its excretion as the main phase I metabolite of MDMA. Copyright © 2016 John Wiley & Sons, Ltd....

  20. Mastering analytical challenges for the characterization of pentacyclic triterpene mono- and diesters of Calendula officinalis flowers by non-aqueous C30 HPLC and hyphenation with APCI-QTOF-MS.

    Science.gov (United States)

    Nicolaus, Christoph; Sievers-Engler, Adrian; Murillo, Renato; D'Ambrosio, Michele; Lämmerhofer, Michael; Merfort, Irmgard

    2016-01-25

    Pentacyclic triterpene mono- and diesters have been isolated from Calendula officinalis flowers. GC-MS, APCI-Exactive Orbitrap HR-MS and NMR allowed to identify the triterpene skeleton in various samples (different triterpene mixtures from Calendula n-hexane extract). NMR provided evidence that triterpene diesters are present in the samples as well. However, the corresponding quasi-molecular ions could not be detected by APCI-Exactive Orbitrap HR-MS. Instability of triterpene diesters and loss of a fatty acid residue, respectively, in the ion-source made their MS detection challenging. Thus, a set of new APCI-QTOF-MS methods (using the TripleTOF 5600+ mass spectrometer) were developed which made it eventually possible to solve this problem and confirm the diester structures by MS via quasi-molecular ion [M+H](+) detection. Direct infusion APCI-QTOF MS experiments in MS/MS high sensitivity scan mode with low collision energy and multi-channel averaging acquisition (MCA) allowed the detection of quasi-molecular ions of triterpene diesters for the first time and unequivocally confirmed the presence of faradiol 3,16-dimyristate and -dipalmitate, as well as the corresponding mixed diesters faradiol 3-myristate,16-palmitate and faradiol 3-palmitate,16-myristate. Preferential loss of the fatty acid in 16-position made it possible to distinguish the mixed diesters by MS/MS spectra. Their chromatographic separations turned out to be challenging due to their bulkiness and extended molecular dimensions. However, separation could be achieved by an uncommon non-aqueous RPLC mode with an in-house synthesized C30 phase. Finally, two (U)HPLC-APCI-QTOF-MS methods with C18- and C30-based non-aqueous RPLC provided suitable, sensitive assays to monitor the presence of monoesters and diesters of various triterpenes (faradiol, maniladiol, arnidiol, arnitriol A and lupane-3β,16β,20-triol esters) in the n-hexane extract of C. officinalis with high mass resolution and good mass accuracy. PMID:26562182

  1. Asymmetric Flow-Field Flow Fractionation Hyphenated ICP-MS as an Alternative to Cloud Point Extraction for Quantification of Silver Nanoparticles and Silver Speciation: Application for Nanoparticles with a Protein Corona.

    Science.gov (United States)

    Mudalige, Thilak K; Qu, Haiou; Linder, Sean W

    2015-07-21

    Production and application of nanoparticles in consumer products is at an all-time high due to the emerging field of nanotechnology. Direct detection and quantification of trace levels of nanoparticles within consumer products is very challenging and problematic. Although multiple methodologies are available for this purpose, each method has its own set of limitations. Herein, we developed an analytical platform consisting of asymmetric flow-field flow fractionation (AF4) coupled with inductively coupled plasma mass spectroscopy (ICP-MS) for the speciation and quantification of silver ions and silver nanoparticles at the ng/kg level (ppt). AF4 is utilized to concentrate the nanoparticles, and ICP-MS acts as the detector. The protein corona that forms upon exposure of nanoparticles to bovine serum albumin was utilized as a nanoparticle stabilization and AF4 recovery enhancement mechanism. Speciation of silver ions and nanoparticles was achieved with the assistance of penicillamine as a complexation ligand. The effect of nanoparticle size, surface coating, and ionization state toward the detection and quantification of the developed methodology was evaluated. The detection limit was found to be 4 ng/kg with the application of a 5 mL sample loop. Further application of this developed methodology on environmentally relevant samples was demonstrated by the analysis of Arkansas River water spiked with silver nanoparticles and nanoparticle spiked into humic acid solution (50 mg/L) at an environmentally relevant level.

  2. 气相色谱-质谱联用法测定川贝母中的挥发性化学成分%HYPHENATED GC-MS DETERMINATION OF VOLATILE CONSTITUENTS IN FRITILLARIA CIRRHOSA D.DON

    Institute of Scientific and Technical Information of China (English)

    李玉美

    2008-01-01

    研究川贝母的挥发性化学成分.川贝母样品经水蒸气蒸馏得挥发油,并用气相色谱一质谱法进行分析,按峰面积归一化法求出挥发性化学成分的相对含量.分离出39个峰,已鉴定了14个化合物,占其挥发油总相对含量的81.92%.已鉴定的化合物主要包括1-十八烯(16.38%),1-十二烯(15.09%),十六烷基一环氧乙烷(11.38%),棕榈醇(10.65%),花生醇(7.95%),9-十八炔酸甲酯(6.94%),n-十六酸(5.41%).

  3. 萃取技术和联用技术在铅的形态分析中的应用%Application of Extraction and Hyphenated Techniques for Lead Speciation in Food and Some other Samples

    Institute of Scientific and Technical Information of China (English)

    陈维; 周耀明; 张倩倩; 杨小弟

    2005-01-01

    铅是环境生物体系和食物中存在的污染元素,其毒性与化学形态密切相关.文章重点概述了国内外近年来萃取技术和联用技术在食品等物质中铅形态分析上的应用进展.

  4. 毛细管电泳-质谱联用技术在环境分析中的应用%Application of Capillary Electrophoresis-mass Spectrometry Hyphenated Technology in Environmental Analysis

    Institute of Scientific and Technical Information of China (English)

    陈祥辉; 付大友; 袁东

    2010-01-01

    毛细管电泳-质谱(CE-MS)联用技术综合了CE的快速、高分离能力与MS强大的鉴定功能等特点,已经成为一种重要的分离分析手段.文章对CE-MS联用的发展、特点及在环境分析领域的应用进展予以综述.

  5. High Performance Liquid Chromatography and Related Hyphenated Techniques for the Speciation Analysis of Mercury%高效液相色谱及其联用技术在汞形态分析中的应用

    Institute of Scientific and Technical Information of China (English)

    梁立娜; 江桂斌

    2002-01-01

    本文对近二十年来高效液相色谱及其联用技术在汞的形态分析中的应用进行了综述.着重讨论了样品的前处理方法,高效液相色谱用于汞化合物的形态分离以及检测器的选择.

  6. On the Use of the Hyphen “-” in The Contemporary Chinese Dictionary%《现代汉语词典》注音中短横“-”的使用问题

    Institute of Scientific and Technical Information of China (English)

    张军; 李战

    2011-01-01

    本文通过全面检视《现代汉语词典》(第5版)的注音拼写情况,发现注音拼写中存在一些与政府政策、法规相抵牾之处,主要表现在两个方面:1.词典内部不一致,自相矛盾;2.应使用短横而未用.

  7. Inductively Coupled Plasma(ICP) Mass Spectrometry(MS) Hyphenated with Atomic Emission Spectrometry(AES) for Simultaneous Determination of Major, Minor and Micro Amounts of Elements in Geochemical Samples

    Institute of Scientific and Technical Information of China (English)

    HUANG Zhen-yu; ZHANG Qin; HU Ke; WU Jian-ling; YANG Peng-yuan

    2005-01-01

    @@ Introduction Geological resource survey demands for determining various constituents including major, minor, micro, trace and ultra-trace levels of elements for preparing the map of resource distribution of our country. As a powerful and popularly used technique for multi-element analysis, inductively coupled plasma(ICP) atomic emission spectrometry (AES) has been applied to this field for a period of time[1-3]. However, ICP spectrometric determination of those micro, trace and ultratrace elements needs enrichment procedures for improving the detection limit, which is unacceptable in case a great mass of samples should be analyzed as that in the task of geological resource survey. On the other hand, although ICP mass spectrometry(MS) is considered the most powerful method for trace elements determination[4,5], it is difficult for ICP-MS to be used to determine the trace and major analytes simultaneously in a spectrum.

  8. Hyphenated Technique of Spectrum Analyzer and Mass Spectrometer in Environmental Samples Analysis%环境样品分析中的光谱-质谱联用技术

    Institute of Scientific and Technical Information of China (English)

    陈润发; 李康柏; 李惠贤

    2016-01-01

    电感耦合等离子体质谱(ICP-MS)是光谱-质谱联用技术的典型代表.文章介绍ICP-MS的基本特性及用途,归纳ICP-MS联用技术的应用拓展,充分体现光谱-质谱联用技术在环境样品分析中的重要地位.

  9. Application of the Solid-Phase Microextraction Chromatography Hyphenated with Mass Spectrometry to the Analysis of Petroluem Content in Water%固相微萃取-色谱/质谱技术分析水中汽油成分

    Institute of Scientific and Technical Information of China (English)

    陈旭东; 周红

    2000-01-01

    @@ 对于样品中有机物的分离,传统的前处理技术有液-液萃取、顶空富集(ACS)、超临界萃取(SPE)和吹扫-捕集法等.这些方法所需样品量较多、耗时长,有些试剂有碍人体健康,并造成环境污染等.

  10. 联用新技术在元素形态分析领域中的应用进展%Applications of new hyphenated techniques in element speciation analysis

    Institute of Scientific and Technical Information of China (English)

    侯建荣; 黄聪; 彭荣飞; 毛新武; 李铁刚

    2013-01-01

    对联用技术在元素形态分析中的应用进行了综述,重点介绍了HPLC-AFS、HPLC-ICP-MS、GC-ICP-MS、CE-ICP-MS等几种联用技术在形态分析中的应用,并对元素形态分析的前景进行了展望.

  11. Recent Progress of Application of FIA in Hyphenation with Instrumental Analysis%流动注射分析法与多种仪器分析联用的进展

    Institute of Scientific and Technical Information of China (English)

    金绍祥

    2009-01-01

    对流动注射分析法(FIA)与多种仪器分析方法,包括分光光度法、电感耦合等离子体原子发射光谱法(ICP-AES)、原子吸收光谱法(AAS)、化学发光法(CL)、荧光光度法、电化学分析法、生物传感器、毛细管电泳、免疫分析法等联用在最近两年中的新进展作了评述,引述文献42篇.

  12. 《现代汉语词典》注音拼写的连写分写问题%Hyphenation of notational phonetic alphabets in The Modern Chinese Dictionary

    Institute of Scientific and Technical Information of China (English)

    张军

    2000-01-01

    @@ 《现代汉语词典》(以下简称《现汉》)1996年出版修订本,“修订工作主要从词语增删、推行规范、增补修正释义、增补用例、完善体例等几个方面进行”.在“推行规范”方面,《现汉》“编写的目……

  13. 联用技术在生物体系化合物分析中的应用进展%APPLICATION ADVANCE OF THE HYPHENATED TECHNIQUE ON BIOSYSTEM COMPOUNDANALYSIS

    Institute of Scientific and Technical Information of China (English)

    汤广宇; 张曦

    2009-01-01

    介绍了目前分离分析生物体系化合物的一般步骤和注意事项.综述了联用技术在生物体系化合物分析中的应用进展情况.展望了联用技术在生物体系化合物分析中的发展方向和应用前景.

  14. 从《现代汉语词典》(第5版)谈成语拼音分连写标准%On Hyphenation of Phonetic Letters of Chinese Idioms in Modern Chinese Dictionary (5th Edition)

    Institute of Scientific and Technical Information of China (English)

    王飙

    2009-01-01

    本文考察了第5版成语拼音标注的修订情况,指出其仍没有妥善解决成语拼音分连写方面的疏漏争矛盾,根源在于编者在古今汉语确定词的两种标准间游移不定、顾此失彼,进而指出应该以古代汉语标准为主给成语分词,并给出了分词标准.

  15. My opinion on hyphen usage prescribed in national standard GB /T 15834-1995%关于GB/T 15834-1995中连接号应用问题之我见

    Institute of Scientific and Technical Information of China (English)

    杨小萍

    2005-01-01

    通过对GB/T15834-1995中关于连接号应用标准的制定及在实际应用中存在问题的分析,提出有关连接号应用的分类原则,进而对其应用类型和应用标准提出修改意见,以达到易学易用、表意明确、避免误用混用的目的.

  16. 在线离子交换-ICP-OES测定水中微量六价铬%The Determination of Trace Chromium (Ⅵ) in Tanning Wasterwater by ICP-OES Hyphenated with On-Line Ion-Exchange

    Institute of Scientific and Technical Information of China (English)

    陈斌; 韩双来

    2014-01-01

    建立了流动注射离子交换预富集与电感耦合等离子体原子发射光谱法(FIA-IE-ICP-OES)测定制革废水中微量六价铬的分析方法,确定了最佳的分析条件,其准确度和精密度较国标方法明显提高,检出限为0.003 mg/L.

  17. Structural changes that accompany the self-assembly of hydrophobins

    NARCIS (Netherlands)

    Vocht, Marcel Leo de

    2001-01-01

    De meeste schimmels groeien in lange draadvormige structuren die schimmeldraden of hyphen genoemd worden. Deze hyphen scheiden aan hun uiteinden zogenaamde hydrofobines uit. Deze klasse eiwitten speelt een belangrijke rol in de groei en ontwikkeling van schimmels. De belangrijkste eigenschap van hyd

  18. Are Flow Injection-based Approaches Suitable for Automated Handling of Solid Samples?

    DEFF Research Database (Denmark)

    Miró, Manuel; Hansen, Elo Harald; Cerdà, Victor

    , multisyringe flow injection, and micro-Lab-on-valve are presented as appealing approaches for on-line handling of solid samples. Special emphasis is given to the capability of flow systems to accommodate sequential extraction protocols for partitioning of trace elements and nutrients in environmental solids (e......Flow-based approaches were originally conceived for liquid-phase analysis, implying that constituents in solid samples generally had to be transferred into the liquid state, via appropriate batch pretreatment procedures, prior to analysis. Yet, in recent years, much effort has been focused...... on the design and characterisation of sample processings units coupled with flowing systems aiming to enable the direct introduction and treatment of solid samples of environmental and agricultural origin in an automated fashion [1]. In this respect, various sample pre-treatment techniques including...

  19. Exploiting flow Injection and sequential injection schemes for trace metal determinations by electrothermal atomic absorption spectrometry

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    in flow injection (FI) or sequential injection (SI) systems, which, in addition to reducing sample and reagent consumption, allow all manipulations to be made on-line under enclosed and strictly controlled conditions, thereby minimizing the risk for contamination from the environment. Various separation...... increased flow resistance. This can, however, to a large extent be alleviated by using countercurrent flow. Besides, the surface properties of the resin might be irreversibly changed after having been subjected to a large number of samples, either due to contamination, deactivation, or even loss of its...... these problems might be readily overcome by using an approach where the ion-exchange material is discarded and renewed after each measuring cycle. Based on the so-called lab-on-valve SI-system, which in its design only consumes very minute amounts of ion-exchange material, the cost per assay is amply compensated...

  20. The Impact of Flow Injection on Modern Chemical Analysis

    DEFF Research Database (Denmark)

    Hansen, Elo Harald

    There is no doubt that Flow Injection Analysis (FIA) has had a profound impact on the ways and means that modern analytical chemical procedures are performed. This is amply reflected in the voluminous scientific literature, which by the middle of 2004 passed more than 14,500 FIA-publications in i......There is no doubt that Flow Injection Analysis (FIA) has had a profound impact on the ways and means that modern analytical chemical procedures are performed. This is amply reflected in the voluminous scientific literature, which by the middle of 2004 passed more than 14,500 FIA...... and preconcentration procedures. In recent years, FIA has been supplemented by Sequential Injection Analysis (SIA) and the Lab-on-Valve (LOV) approach. Following a brief historic introduction and an account of the impact of FIA in academia, the lecture will describe these two new generations of FIA, accompanied...

  1. Flow Injection Analysis in Industrial Biotechnology

    DEFF Research Database (Denmark)

    Hansen, Elo Harald; Miró, Manuel

    2009-01-01

    Flow injection analysis (FIA) is an analytical chemical continuous-flow (CF) method which in contrast to traditional CF-procedures does not rely on complete physical mixing (homogenisation) of the sample and the reagent(s) or on attaining chemical equilibria of the chemical reactions involved...... and operational characteristics of FIA are first outlined, and then its downscaled/miniaturized sequels, that is, sequential injection analysis (SIA) and lab-on-valve (LOV), are detailed. Thus, in SIA the sample and reagents are, via the use of a multiposition valve and an attached syringe pump operated under...... live cells, can be handled and utilized as demonstrated. Because the syringe pump in SIA and LOV can be used for accurately aspirating, propelling or even stopping the flow, these modi operandi allow fully to exploit the interplay between the kinetics and the thermodynamics of the chemical reactions...

  2. Distress and Fury: The Governor-General Award Winner Fred Wah and the Strategy of Ethnic Hyphenation%困惑和愤怒——评加拿大总督奖作家Fred Wah和少数族裔作家的连接号策略

    Institute of Scientific and Technical Information of China (English)

    赵庆庆

    2006-01-01

    本文探讨了加拿大总督奖作家弗雷德·华(Fred Wah)的获奖传记小说(Diamond Grill),并结合其文论,探讨了自名的困惑、文本的愤怒和少数族裔作家的连接号策略这三大相关论题,得出少数族裔作家必须把多元文化和强势文化的冲突化为自身价值才可生存的结论.

  3. Application of Hyphenation of HPLC and ICP-MS to Water Analysis%高效液相色谱-电感耦合等离子体质谱联用技术在水质分析中的应用

    Institute of Scientific and Technical Information of China (English)

    苏宇亮

    2009-01-01

    对高效液相色谱-电感耦合等离子体质谱联用技术在水质分析中的应用作了评述,对高效液相色谱-电感耦合等离子体质谱联用技术的发展前景作了展望.引用文献48篇.

  4. Perspectives on Norwegian-Russian energy cooperation

    Energy Technology Data Exchange (ETDEWEB)

    Bourmistrov, Anatoli; Mellemvik, Frode; Vasiliev, Sergey Vasiliev (eds.)

    2011-07-01

    Review from publisher: Perspectives on Norwegian#Hyphen#Russian Energy Cooperation, September 2011 NAREC : Norwegian#Hyphen# Russian Education and Research Consortium for International Business Development in the field of Energy The book illustrates the kind of knowledge and competence possessed by the NAREC partner academic institutions: Part I highlights and discusses opportunities and barriers for the Norwegian#Hyphen#Russian energy cooperation in the High North. Part II considers and exemplifies the High North as an arena for increasing modernization and innovations. Part III devoted to advanced technologies for developing the High North.(Author)

  5. ACTINET-I3 Summer School on Analytical Innovation in the field of actinide recycling - Slides of the presentations

    International Nuclear Information System (INIS)

    This conference dealt with 3 main topics: analytical innovation in separation processes (hyphenated techniques, analytical chips,...), actinide recycling (extraction, interfaces, processes,...) and chemistry and thermodynamics of actinides. This document is composed of the slides of the presentations

  6. On-line sample processing methods in flow analysis

    DEFF Research Database (Denmark)

    Miró, Manuel; Hansen, Elo Harald

    2008-01-01

    -line dilution, derivatization, separation and preconcentration methods encompassing solid reactors, solvent extraction, sorbent extraction, precipitation/coprecipitation, hydride/vapor generation and digestion/leaching protocols as hyphenated to a plethora of detection devices is discussed in detail...

  7. Raman spectroscopy in pharmaceutical product design

    DEFF Research Database (Denmark)

    Paudel, Amrit; Raijada, Dhara; Rantanen, Jukka

    2015-01-01

    molecular-based drug discovery, design of innovative drug delivery systems and quality control of finished products. This review presents concise accounts of various conventional and emerging Raman instrumentations including associated hyphenated tools of pharmaceutical interest. Moreover, relevant...

  8. Normal Pancreas Anatomy

    Science.gov (United States)

    ... hyphen, e.g. -historical Searches are case-insensitive Pancreas Anatomy Add to My Pictures View /Download : Small: ... 1586x1534 View Download Large: 3172x3068 View Download Title: Pancreas Anatomy Description: Anatomy of the pancreas; drawing shows ...

  9. Mecánica estadística, neodarwinismo y la prefiguración de las ciencias de la complejidad

    OpenAIRE

    Andrade Luis Eugenio

    2009-01-01

  1. Uma reflexão teórica da Doença Pulmonar Obstrutiva Crônica (DPOC)

    OpenAIRE

    Crhis Netto de Brum; Tassiane Ferreira Langendorf

    2009-01-01

  1. State, nation and immigration: the national order facing the challenge of immigration Estado, nación e inmigración. El orden nacional ante el desafío de la inmigración

    OpenAIRE

    Abdelmalek Sayad

    2008-01-01

    A CONVERSÃO DE CONHECIMENTO ATRAVÉS DO “LEARNING BY HIRING” NO PROGRAMA EMBRAER 170/190

    OpenAIRE

    Ricardo Gentil Peixoto da Costa; Henrique Pazos Siqueira Boclin; Luiz Alberto Nascimento Campos Filho

    2008-01-01

  1. Analysis of nanoparticles using the ICAP Q ICP-MS

    DEFF Research Database (Denmark)

    Kutscher, Daniel; McSheehy-Ducos, Shona; Lindemann, Torsten;

    2014-01-01

    The analysis of Nanoparticles (NPs) has become one of the hot topics in analytical chemistry. However, detailed knowledge about potential risks or hazards is still unavailable. Two approaches have been developed in recent years using ICP-MS as a detection system: hyphenation of an appropriate...

  2. Genes for 7S RNAs can replace the gene for 4.5S RNA in growth of Escherichia coli

    DEFF Research Database (Denmark)

    Brown, S

    1991-01-01

    4.5S RNAs of eubacteria and 7S RNAs of archaebacteria and eukaryotes exist in a hairpin conformation. The apex of this hairpin displays structural and sequence similarities among both 4.5S and 7S RNAs. Furthermore, a hyphenated sequence of 16 nucleotides is conserved in all eubacterial 4.5S RNAs...

  3. Alkaloid analysis by high-performance liquid chromatography-solid phase extraction-nuclear magnetic resonance

    DEFF Research Database (Denmark)

    Johansen, Kenneth; Ebild, S.J.; Christensen, S.B.;

    2012-01-01

    The hyphenated technique HPLC-SPE-NMR is an important tool for rapid dereplication of complex mixtures of in particular small molecules and has been successfully employed in natural product research. However, positively charged alkaloids at low pH are often poorly trapped on the generally used SP...

  4. Instrument and process independent binning and baseline correction methods for liquid chromatography-high resolution-mass spectrometry deconvolution

    NARCIS (Netherlands)

    Krishnan, S.; Vogels, J.T.W.E.; Coulier, L.; Bas, R.C.; Hendriks, M.W.B.; Hankemeier, T.; Thissen, U.

    2012-01-01

    Setting appropriate bin sizes to aggregate hyphenated high-resolution mass spectrometry data, belonging to similar mass over charge (m/. z) channels, is vital to metabolite quantification and further identification. In a high-resolution mass spectrometer when mass accuracy (ppm) varies as a function

  5. Orthographe: la fin d'un tabou (Orthography: The End of a Taboo).

    Science.gov (United States)

    Olivieri, Claude

    1990-01-01

    Significant features of the official October 1990 orthographic reforms in French are outlined and their pedagogical implications are discussed briefly. The changes, primarily simplifications and not major changes, affect use of the hyphen, plurals, diacritical markings, verb tenses, and correction of anomalies. (MSE)

  6. Cataluminescence-based sensors: principle, instrument and application.

    Science.gov (United States)

    Tang, Fei; Guo, Cheng'an; Chen, Jin; Zhang, Xinrong; Zhang, Sichun; Wang, Xiaohao

    2015-11-01

    The cataluminescence (CTL)-based sensor is a new promising type of chemical transducer, and has attracted much attention of researchers for its potential versatile applications in public safety, emission control and environmental protection. In this review, we briefly introduce the development history of CTL-based sensors and summarize existing explanations of the CTL reaction mechanism as well as three research strategies for mechanism the CTL mechanism. In the following, all the function units of a typical CTL-based sensor system are described and the investigation of the sensor materials. CTL-based sensor arrays, are discussed in detail. We classify the recent novel hyphenated techniques based on CTL coupled to other analysis techniques into the preconcentration-CTL hyphenated technique, nebulization-CTL hyphenated technique, plasma-assisted CTL technique and tandem CTL technique according to the type of analysis combined with CTL and provide a detailed account of novel hyphenated techniques. Owing to the appearance of these novel techniques, the application range of CTL has been expanded as well as the sensitivity and selectivity of CTL system has been greatly improved. Finally, the applications of CTL-based sensor and sensor arrays in the last several years are classified and summarized.

  7. Eletroforese capilar acoplada à espectrometria com plasma: uma ferramenta eficiente para a especiação Capillary electrophoresis coupled to plasma spectrometry: an efficient tool for speciation

    Directory of Open Access Journals (Sweden)

    Ana Paula G. Gervasio

    2003-01-01

    Full Text Available The most important features of the CE-ICP hyphenation, as well as its advantages and drawbacks as a tool for speciation are discussed. The fundamental principles of capillary electrophoresis and inductively coupled plasma mass spectrometry are also presented. Some applications involving different designs proposed in the literature to couple CE and ICP system for elemental speciation are reviewed.

  8. Identification of the major constituents of Hypericum perforatum by LC/SPE/NMR and/or LC/MS.

    NARCIS (Netherlands)

    Tatsis, E.C.; Boeren, J.A.; Exarchou, V.; Troganis, A.N.; Vervoort, J.J.M.; Gerothanassis, I.P.

    2007-01-01

    The newly established hyphenated instrumentation of LC/DAD/SPE/NMR and LC/UV/(ESI)MS techniques have been applied for separation and structure verification of the major known constituents present in Greek Hypericum perforatum extracts. The chromatographic separation was performed on a C18 column. Ac

  9. Automated sequential injection-microcolumn approach with on-line flame atomic absorption spectrometric detection for implementing metal fractionation schemes of homogeneous and non-homogeneous solid samples of environmental interest

    DEFF Research Database (Denmark)

    Chomchoei, Roongrat; Miró, Manuel; Hansen, Elo Harald;

    2005-01-01

    spectrometric detection and used for the determination of Cu as a model analyte, the potentials of this novel hyphenated approach are demonstrated by the ability of handling up to 300 mg sample of a nonhomogeneous sewage amended soil (viz., CRM 483). The three steps of the endorsed Standards, Measurements...

  10. MADE IN CHINA:AMERICAN DREAMS

    Institute of Scientific and Technical Information of China (English)

    2006-01-01

    "Made in China." It's a little tag, which, discovered within an otherwise sharp pair of shoes or leather jacket, not so long ago might have prompted sneering in America. "American." It's a powerful word with an aura further strengthened when invisibly hyphenated to "Dream." Yet as homegrown American companies like Home

  11. Punctuation Potpourri. An Office Education Mini Curriculum Manual on Other Punctuation Marks.

    Science.gov (United States)

    Hawkinson, Bruce

    One in a series of ten mini-manuals on office communication proofreading, this booklet for business and office students provides instruction in the use of apostrophes, quotes, italics, hyphens, brackets, ellipsis dots, leader dots, bullets, superscripts, and subscripts. Included are terminal and specific objectives, punctuation rules and related…

  12. The Development of Whole-Word Representations in Compound Word Processing: Evidence from Eye Fixation Patterns of Elementary School Children

    Science.gov (United States)

    Haikio, Tuomo; Bertram, Raymond; Hyona, Jukka

    2011-01-01

    The role of morphology in reading development was examined by measuring participants' eye movements while they read sentences containing either a hyphenated (e.g., "ulko-ovi" "front door") or concatenated (e.g., "autopeli" "racing game") compound. The participants were Finnish second, fourth, and sixth graders (aged 8, 10, and 12 years,…

  13. Eletroforese capilar acoplada à espectrometria com plasma: uma ferramenta eficiente para a especiação Capillary electrophoresis coupled to plasma spectrometry: an efficient tool for speciation

    OpenAIRE

    Ana Paula G. Gervasio; André F. Lavorante; Maria Carolina B. Moraes; Maria Fernanda Giné; Carlos E. S. Miranda; Emanuel Carrilho

    2003-01-01

    The most important features of the CE-ICP hyphenation, as well as its advantages and drawbacks as a tool for speciation are discussed. The fundamental principles of capillary electrophoresis and inductively coupled plasma mass spectrometry are also presented. Some applications involving different designs proposed in the literature to couple CE and ICP system for elemental speciation are reviewed.

  14. On-line liquid phase micro-extraction based on drop-in-plug sequential injection lab-at-valve platform for metal determination

    International Nuclear Information System (INIS)

    Highlights: ► Drop-in-plug micro-extraction based on SI-LAV platform for metal preconcentration. ► Automatic liquid phase micro-extraction coupled with FAAS. ► Organic solvents with density higher than water are used. ► Lead determination in environmental water and urine samples. -- Abstract: A novel automatic on-line liquid phase micro-extraction method based on drop-in-plug sequential injection lab-at-valve (LAV) platform was proposed for metal preconcentration and determination. A flow-through micro-extraction chamber mounted at the selection valve was adopted without the need of sophisticated lab-on-valve components. Coupled to flame atomic absorption spectrometry (FAAS), the potential of this lab-at-valve scheme is demonstrated for trace lead determination in environmental and biological water samples. A hydrophobic complex of lead with ammonium pyrrolidine dithiocarbamate (APDC) was formed on-line and subsequently extracted into an 80 μL plug of chloroform. The extraction procedure was performed by forming micro-droplets of aqueous phase into the plug of the extractant. All critical parameters that affect the efficiency of the system were studied and optimized. The proposed method offered good performance characteristics and high preconcentration ratios. For 10 mL sample consumption an enhancement factor of 125 was obtained. The detection limit was 1.8 μg L−1 and the precision expressed as relative standard deviation (RSD) at 50.0 μg L−1 of lead was 2.9%. The proposed method was evaluated by analyzing certified reference materials and applied for lead determination in natural waters and urine samples

  15. MSFIA-LOV system for (226)Ra isolation and pre-concentration from water samples previous radiometric detection.

    Science.gov (United States)

    Rodríguez, Rogelio; Borràs, Antoni; Leal, Luz; Cerdà, Víctor; Ferrer, Laura

    2016-03-10

    An automatic system based on multisyringe flow injection analysis (MSFIA) and lab-on-valve (LOV) flow techniques for separation and pre-concentration of (226)Ra from drinking and natural water samples has been developed. The analytical protocol combines two different procedures: the Ra adsorption on MnO2 and the BaSO4 co-precipitation, achieving more selectivity especially in water samples with low radium levels. Radium is adsorbed on MnO2 deposited on macroporous of bead cellulose. Then, it is eluted with hydroxylamine to transform insoluble MnO2 to soluble Mn(II) thus freeing Ra, which is then coprecipitated with BaSO4. The (226)Ra can be directly detected in off-line mode using a low background proportional counter (LBPC) or through a liquid scintillation counter (LSC), after performing an on-line coprecipitate dissolution. Thus, the versatility of the proposed system allows the selection of the radiometric detection technique depending on the detector availability or the required response efficiency (sample number vs. response time and limit of detection). The MSFIA-LOV system improves the precision (1.7% RSD), and the extraction frequency (up to 3 h(-1)). Besides, it has been satisfactorily applied to different types of water matrices (tap, mineral, well and sea water). The (226)Ra minimum detectable activities (LSC: 0.004 Bq L(-1); LBPC: 0.02 Bq L(-1)) attained by this system allow to reach the guidance values proposed by the relevant international agencies e.g. WHO, EPA and EC. PMID:26893088

  16. Gas Chromatography/Atmospheric Pressure Chemical Ionization-Fourier Transform Ion Cyclotron Resonance Mass Spectrometry of Pyrolysis Oil from German Brown Coal

    Directory of Open Access Journals (Sweden)

    Jan Zuber

    2016-01-01

    Full Text Available Pyrolysis oil from the slow pyrolysis of German brown coal from Schöningen, obtained at a temperature of 500°C, was separated and analyzed using hyphenation of gas chromatography with an atmospheric pressure chemical ionization source operated in negative ion mode and Fourier transform ion cyclotron resonance mass spectrometry (GC-APCI-FT-ICR-MS. Development of this ultrahigh-resolving analysis method is described, that is, optimization of specific GC and APCI parameters and performed data processing. The advantages of GC-APCI-FT-ICR-MS hyphenation, for example, soft ionization, ultrahigh-resolving detection, and most important isomer separation, were demonstrated for the sample liquid. For instance, it was possible to separate and identify nine different propylphenol, ethylmethylphenol, and trimethylphenol isomers. Furthermore, homologous series of different acids, for example, alkyl and alkylene carboxylic acids, were verified, as well as homologous series of alkyl phenols, alkyl dihydroxy benzenes, and alkoxy alkyl phenols.

  17. From retrospective assessment to prospective decisions in natural product isolation

    DEFF Research Database (Denmark)

    Johansen, Kenneth T; Wubshet, Sileshi G; Nyberg, Nils T;

    2011-01-01

    An extract of Carthamus oxyacantha (wild safflower) was investigated using two approaches: a traditional, nontarget fractionation by VLC and HPLC, and the hyphenated technique HPLC-PDA-HRMS-SPE-NMR followed by targeted isolation of selected constituents for inclusion in a screening library of pure...... natural products. While the nontarget fractionation involved considerable time spent on pursuing fractions containing well-known or undesired compounds, the hyphenated analysis was considerably faster and required less solvent and other consumables. The results were used to design and execute an optimized......, HPLC-HRMS-guided, targeted isolation scheme aiming exclusively at a series of identified spiro compounds. Thus, HPLC-PDA-HRMS-SPE-NMR is a dereplication technique of choice, allowing economical acquisition of comprehensive data about compounds in crude extracts, which can be used for rational...

  18. Erotic(izing Cubans

    Directory of Open Access Journals (Sweden)

    Virginia R. Domínguez

    1996-07-01

    Full Text Available [First paragraph] Sugar's Secrets: Race and the Erotics of Cuban Nationalism. VERA M. KUTZINSKI. Charlottesville: University Press of Virginia, 1993. xvii + 287 pp. (Cloth US$ 40.00, Paper US$ 17.95 Life on the Hyphen: The Cuban-American Way. GUSTAVO PÉREZ FlRMAT. Austin: University of Texas Press, 1994. xii + 217 pp. (Cloth US$ 30.00, Paper US$ 12.95 When a country is subjected to as much external political and ideological scrutiny as Cuba in the post-Batista years, scholarly explorations of something other than its foreign policy, its political economy, and its human rights abuses provide a breath of fresh air. But I am struck by the other things Sugar's Secrets and Life on the Hyphen have in common and how suspicious I am of their commonalities.

  19. 色谱联用技术的研究进展%Research Progress of Hypenated Chromatographic Techniques

    Institute of Scientific and Technical Information of China (English)

    杨洁; 索习东

    2012-01-01

    综述了色谱联用技术的发展概况及其在各种研究中的应用和薪进展,同时指出随着色谱联用技术的不断发展,各种新型色谱技术在现代研究中将有更大的发展空间与应用前景。%This article summarized the development of hyphenated Chromatography would techniques and its applications and new developments in various studies. Meanwhile it indicated that there would be greater room and application prospects for new types of chromatographic techniques in modern researches with the continuous development of hyphenated Chromatographic techniques.

  20. Intersubjective relation: change alternative for the human health professions

    Directory of Open Access Journals (Sweden)

    Maria C. Chapela M

    2009-05-01

    Full Text Available Objectives: 1. To exemplify the relationships between changes in the body inscriptions of people exposed to professional health services and the inter-subjective hyphens occurring in those relationships. 2. To identify in those relationships some components of subordination and autonomy. Methodology: here I present one aspect of a critical qualitative case study of a health promotion intervention. Results: the examples provided show changes in the body inscriptions as a product of capital recuperation processes that took part during the intervention. Conclusions: in the particular characteristics of the inter-subjective hyphen unavoidable in the health profession practice, there are subordination and autonomy possibilities. A critical qualitative inquiry perspective can not just improve the understanding of the social determinants of health and subjects’ body inscriptions, but also may help to search for new health concepts and to transform practices which are undermining the capacity of subject to produce their spaces and develop their ethic capacity.

  1. Gas Chromatography/Atmospheric Pressure Chemical Ionization-Fourier Transform Ion Cyclotron Resonance Mass Spectrometry of Pyrolysis Oil from German Brown Coal.

    Science.gov (United States)

    Zuber, Jan; Kroll, Marius M; Rathsack, Philipp; Otto, Matthias

    2016-01-01

    Pyrolysis oil from the slow pyrolysis of German brown coal from Schöningen, obtained at a temperature of 500°C, was separated and analyzed using hyphenation of gas chromatography with an atmospheric pressure chemical ionization source operated in negative ion mode and Fourier transform ion cyclotron resonance mass spectrometry (GC-APCI-FT-ICR-MS). Development of this ultrahigh-resolving analysis method is described, that is, optimization of specific GC and APCI parameters and performed data processing. The advantages of GC-APCI-FT-ICR-MS hyphenation, for example, soft ionization, ultrahigh-resolving detection, and most important isomer separation, were demonstrated for the sample liquid. For instance, it was possible to separate and identify nine different propylphenol, ethylmethylphenol, and trimethylphenol isomers. Furthermore, homologous series of different acids, for example, alkyl and alkylene carboxylic acids, were verified, as well as homologous series of alkyl phenols, alkyl dihydroxy benzenes, and alkoxy alkyl phenols. PMID:27066076

  2. New Oxford style manual

    CERN Document Server

    2012-01-01

    The New Oxford Style Manual brings together two essential reference works in a single volume: New Hart's Rules and the New Oxford Dictionary for Writers and Editors. New Hart's Rules, Oxford's definitive guide to style, consists of 20 chapters that provide authoritative and expert advice on how to prepare copy for publication. Topics covered include how to use italic, roman, and other type treatments, numbers and dates, law and legal references, illustrations, notes and references, and bibliographies. The guidelines are complemented by the New Oxford Dictionary for Writers and Editors, which features 25,000 alphabetically arranged entries giving authoritative advice on those words and names which raise questions time and time again because of spelling, capitalization, hyphenation, or cultural and historical context. Entries give full coverage of recommended spellings, variant forms, confusable words, hyphenation, capitalization, foreign and specialist terms, proper names, and abbreviations. The dictionary a...

  3. Direct Analysis of Oil Additives by High-Field Asymmetric Waveform Ion Mobility Spectrometry-Mass Spectrometry Combined with Electrospray Ionization and Desorption Electrospray Ionization.

    Science.gov (United States)

    Da Costa, Caitlyn; Turner, Matthew; Reynolds, James C; Whitmarsh, Samuel; Lynch, Tom; Creaser, Colin S

    2016-02-16

    The analysis of corrosion inhibitors in the presence and absence of an oil matrix is reported using electrospray ionization (ESI) and desorption electrospray ionization (DESI), hyphenated with miniaturized high-field asymmetric waveform ion mobility spectrometry (FAIMS) and mass spectrometry (MS). The target analytes were successfully ionized in solution by ESI and directly from steel surfaces using DESI ambient ionization at levels ≥0.0004% w/w (4 ppm) in oil. Differences in the mass spectral profiles observed for the additive/oil mixture are attributed to differences between the ESI and DESI ionization processes. The use of FAIMS improved selectivity for ESI generated analyte ions through reduction in the chemical noise resulting from the oil matrix. DESI enabled the direct, rapid, native state interrogation of oil samples on steel surfaces without sample pretreatment, and the hyphenation of DESI with the miniaturized FAIMS enhanced the relative analyte responses of the surface-active corrosion inhibitors. PMID:26780580

  4. Egg White Protein-Bonded Columns and Their Applications%蛋清蛋白质键合柱及其应用

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    Egg white protein-bonded columns were developed for HPLC. These columns can be used under aqueous mobile phase and separate various kinds of drug enantiomers. Hyphenated techniques using protein-bonded columns with LC/MS and/or column switching have been recognized as integral methods in pharmaceutical research to analyze drug enantiomers. Therefore, these methods are very useful for research fields of pharmacokinetics and pharmacology.

  5. Development of LC/MS techniques for plant and drug metabolism studies

    OpenAIRE

    Petsalo, A. (Aleksanteri)

    2011-01-01

    Abstract Liquid chromatography (LC) combined with mass spectrometry (MS) is a powerful tool for qualitative and quantitative analytics of organic molecules from various matrices, and the use of this hyphenated technique is very common in bioanalytical laboratories. In this study, LC/MS methods and the required sample preparation applications were developed for plant flavonoid and drug metabolism studies. The main focus was in developing methods to be used during cytochrome P450 (CYP) -spe...

  6. High-performance thin layer chromatography: A powerful analytical technique in pharmaceutical drug discovery

    OpenAIRE

    Attimarad, Mahesh; Ahmed, K. K. Mueen; Aldhubaib, Bandar E.; Harsha, Sree

    2011-01-01

    Analysis of pharmaceutical and natural compounds and newer drugs is commonly used in all the stages of drug discovery and development process. High-performance thin layer chromatography is one of the sophisticated instrumental techniques based on the full capabilities of thin layer chromatography. The advantages of automation, scanning, full optimization, selective detection principle, minimum sample preparation, hyphenation, and so on enable it to be a powerful analytical tool for chromatogr...

  7. Molecular-level investigation on electrochemical interfaces by Raman spectroscopy

    Institute of Scientific and Technical Information of China (English)

    TIAN, Zhong-Qun; REN, Bin

    2000-01-01

    The structure and dynamics of electrode/liquid interfaces play an increasingly important role in electrochemistry. Raman spectroscopy is capable of providing detailed structural information at molecular level and new insight into the interfacial structure, adsorption, reaction, electrocatalysis and corrosion. In this account we will summarize some progresses of surface Raman spectroscopy in the study of electrochemical interfaces, mainly based on our group's work, laying emphasis on the detection sensitivity, spectral resolution, time resolution and spatial resolution as well as the hyphenated technique.

  8. Aspects of recent developments in analytical chemometrics

    Institute of Scientific and Technical Information of China (English)

    LIANG; Yizeng; WU; Hailong; SHEN; Guoli; JIANG; Jianhui; LIANG; Sheng

    2006-01-01

    Some aspects of recent developments in analytical chemometrics are discussed, in particular the developments viewed from the angle of the research efforts undertaken in authors' laboratories. The topics concerned include resolution of high-order chemical data, morphological theory and methodology for chemical signal processing, multivariate calibration and chemical pattern recognition for solving complex chemical problems, and resolution of two-way chemical data from hyphenated chromatographic instruments.

  9. Soziologie und Ökonomik: Betrachtungen über Konvergenzen und Divergenzen

    OpenAIRE

    Bögenhold, Dieter

    2013-01-01

    During the last century, the question of the relationship of sociology and economics has come up again and again. The explosion of material in sociology and in different fields of economics has given rise to specialisation processes within the subjects. The disciplines have multiplied in both the horizontal and vertical perspective, and sub-subjects (sometimes referred to as hyphenated subjects (Bindestrichfächer) in German) have emerged, which provide their own universes of discourse, each w...

  10. Chemical Characterization of Fruit Wine Made from Oblačinska Sour Cherry

    OpenAIRE

    Milica Pantelić; Dragana Dabić; Saša Matijašević; Sonja Davidović; Biljana Dojčinović; Dušanka Milojković-Opsenica; Živoslav Tešić; Maja Natić

    2014-01-01

    This paper was aimed at characterizing the wine obtained from Oblačinska, a native sour cherry cultivar. To the best of our knowledge, this is the first paper with the most comprehensive information on chemical characterization of Oblačinska sour cherry wine. The chemical composition was characterized by hyphenated chromatographic methods and traditional analytical techniques. A total of 24 compounds were quantified using the available standards and another 22 phenolic compounds were identifi...

  11. Discovering new natural products directly from crude extracts by HPLC-SPE-NMR: chinane diterpenes in Harpagophytum procumbens.

    Science.gov (United States)

    Clarkson, Cailean; Staerk, Dan; Hansen, Steen Honoré; Smith, Peter J; Jaroszewski, Jerzy W

    2006-04-01

    HPLC-SPE-NMR experiments with crude extracts of Harpagophytum procumbens allowed the rapid identification of novel, unstable chinane-type tricyclic diterpenes (1 and 2), along with numerous other constituents. Dramatic sensitivity gains achieved with this novel hyphenated technique establish a new paradigm in natural products research: rapid and rigorous structure determination of multiple extract components, including minor components, without preparative-scale isolation. PMID:16643019

  12. A neuron-in-capillary platform for facile collection and mass spectrometric characterization of a secreted neuropeptide

    OpenAIRE

    Chang Young Lee; Yi Fan; Rubakhin, Stanislav S.; Sook Yoon; Sweedler, Jonathan V.

    2016-01-01

    The integration of microfluidic devices—which efficiently handle small liquid volumes—with separations/mass spectrometry (MS) is an effective approach for profiling the neurochemistry occurring in selected neurons. Interfacing the microfluidic cell culture to the mass spectrometer is challenging because of geometric and scaling issues. Here we demonstrate the hyphenation of a neuron-in-capillary platform to a solid phase extraction device and off-line MS. A primary neuronal culture of Aplysia...

  13. Application of Pyrolysis–Gas Chromatography– Mass Spectrometry for the Identification of Polymeric Materials

    OpenAIRE

    Kusch, Peter; Knupp, Gerd (Prof. Dr.); Fink, Wolfgang; Schroeder-Obst, Dorothee (Prof. Dr.); Obst, Volker (Dr.); Steinhaus, Johannes (Ph.D.)

    2014-01-01

    Analytical pyrolysis technique hyphenated to gas chromatography/mass spectrometry (Py-GC/MS) has extended the range of possible tools for characterization of synthetic polymers/copolymers. Pyrolysis involves thermal fragmentation of the analytical sample at elevated temperature between 500 and 1400 °C. In the presence of an inert gas, reproducible decomposition products characteristic for the original polymer/copolymer sample are formed. The pyrolysis products are chromatographically separate...

  14. Zinc and iron speciation in the cereal grain

    OpenAIRE

    Schjoerring, Jan K.; Persson, Daniel P.; Hansen, Thomas H.; Laursen, Kristian H; Husted, Søren

    2009-01-01

    Phytic acid and proteins are believed to be important for the distribution and bio-availability of zinc and iron in the cereal grain, but little quantitative information is available on the relative importance of different organic ligands. We have used several chromatographic techniques including size exclusion chromatography (SEC) hyphenated to ICP-MS to analyse the molecular speciation of Fe and Zn in tissues of barley and rice seeds. The majority of Fe in barley embryos co-eluted with P as...

  15. Research Progress in Coupled Process of Fenton Oxidation Technology with Other Technologys to Treat Wastewater%Fenton氧化技术与其他方法联用在废水处理方面的研究进展

    Institute of Scientific and Technical Information of China (English)

    王鹏

    2011-01-01

    The hyphenated methods between Fenton oxidation technology and other technologys are reviewed. The characteristics and present state of applications of the adsorption - Fenton oxidation technology,coagulation- Fenton oxidation technology,microwave- Fenton oxidation technology, biological methods -Fenton oxidation technology are explored the places of the hyphenated methods which we can improve are point out. In addition, the prospect of hyphenated methods is predicted.%综述了近些年Fenton氧化技术与其他方法联用在处理难降解有机废水方面的研究进展,探讨了吸附-Fenton氧化技术、混凝-Fenton氧化技术、微波-Fenton氧化技术、生物方法-Fenton氧化技术的特点及其应用研究现状,指出了这些联用技术可改进的地方。此外,展望了联用方法的发展趋势。

  16. Truth Telling, Companionship, and Witness: An Agenda for Narrative Ethics.

    Science.gov (United States)

    Frank, Arthur W

    2016-05-01

    Narrative ethics holds that if you ask someone what goodness is, as a basis of action, most people will first appeal to various abstractions, each of which can be defined only by other abstractions that in turn require further definition. If you persist in asking what each of these abstractions actually means, eventually that person will have to tell you a story and expect you to recognize goodness in the story. Goodness and badness need stories to make them thinkable and to translate them into individual and collective actions. Yet after more than two decades of considering the issue, I do not believe that a collection of stories can by itself guide actions in ways that are sufficient to respond to ethical troubles in institutional settings. The question will always remain open for me, but my present belief is that narrative bioethics is always hyphenated, in the sense that guidance from stories needs to be allied with other ethical guidance. Each side of the hyphen qualifies the other side. The hyphenation I will argue for in this essay is "narrative-deontology."

  17. Direct analysis in real time - high resolution mass spectrometry (DART-HRMS): a high throughput strategy for identification and quantification of anabolic steroid esters.

    Science.gov (United States)

    Doué, Mickael; Dervilly-Pinel, Gaud; Pouponneau, Karinne; Monteau, Fabrice; Le Bizec, Bruno

    2015-07-01

    High throughput screening is essential for doping, forensic, and food safety laboratories. While hyphenated chromatography-mass spectrometry (MS) remains the approach of choice, recent ambient MS techniques, such as direct analysis in real time (DART), offer more rapid and more versatile strategies and thus gain in popularity. In this study, the potential of DART hyphenated with Orbitrap-MS for fast identification and quantification of 21 anabolic steroid esters has been evaluated. Direct analysis in high resolution scan mode allowed steroid esters screening by accurate mass measurement (Resolution = 60 000 and mass error  0.99), dynamic range (from 1 to 1000 ng mL(-1) ), bias (<10%), sensitivity (1 ng mL(-1) ), repeatability and reproducibility (RSD < 20%) were evaluated as similar to those obtained with hyphenated chromatography-mass spectrometry techniques. This innovative high throughput approach was successfully applied for the characterization of oily commercial preparations, and thus fits the needs of the competent authorities in the fight against forbidden or counterfeited substances.

  18. Truth Telling, Companionship, and Witness: An Agenda for Narrative Ethics.

    Science.gov (United States)

    Frank, Arthur W

    2016-05-01

    Narrative ethics holds that if you ask someone what goodness is, as a basis of action, most people will first appeal to various abstractions, each of which can be defined only by other abstractions that in turn require further definition. If you persist in asking what each of these abstractions actually means, eventually that person will have to tell you a story and expect you to recognize goodness in the story. Goodness and badness need stories to make them thinkable and to translate them into individual and collective actions. Yet after more than two decades of considering the issue, I do not believe that a collection of stories can by itself guide actions in ways that are sufficient to respond to ethical troubles in institutional settings. The question will always remain open for me, but my present belief is that narrative bioethics is always hyphenated, in the sense that guidance from stories needs to be allied with other ethical guidance. Each side of the hyphen qualifies the other side. The hyphenation I will argue for in this essay is "narrative-deontology." PMID:27150414

  19. Bead-Based Microfluidic Sediment Analogues: Fabrication and Colloid Transport.

    Science.gov (United States)

    Guo, Yang; Huang, Jingwei; Xiao, Feng; Yin, Xiaolong; Chun, Jaehun; Um, Wooyong; Neeves, Keith B; Wu, Ning

    2016-09-13

    Mobile colloids can act as carriers for low-solubility contaminants in the environment. However, the dominant mechanism for this colloid-facilitated transport of chemicals is unclear. Therefore, we developed a bead-based microfluidic platform of sediment analogues and measured both single and population transport of model colloids. The porous medium is assembled through a bead-by-bead injection method. This approach has the versatility to build both electrostatically homogeneous and heterogeneous media at the pore scale. A T-junction at the exit also allowed for encapsulation and enumeration of colloids effluent at single particle resolution to give population dynamics. Tortuosity calculated from pore-scale trajectory analysis and its comparison with lattice Boltzmann simulations revealed that transport of colloids was influenced by the size exclusion effect. The porous media packed by positively and negatively charged beads into two layers showed distinctive colloidal particle retention and significant remobilization and re-adsorption of particles during water flushing. We demonstrated the potential of our method to fabricate porous media with surface heterogeneities at the pore scale. With both single and population dynamics measurement, our platform has the potential to connect pore-scale and macroscale colloid transport on a lab scale and to quantify the impact of grain surface heterogeneities that are natural in the subsurface environment. PMID:27548505

  20. Ndel1-derived peptides modulate bidirectional transport of injected beads in the squid giant axon

    Directory of Open Access Journals (Sweden)

    Michal Segal

    2012-01-01

    Bidirectional transport is a key issue in cellular biology. It requires coordination between microtubule-associated molecular motors that work in opposing directions. The major retrograde and anterograde motors involved in bidirectional transport are cytoplasmic dynein and conventional kinesin, respectively. It is clear that failures in molecular motor activity bear severe consequences, especially in the nervous system. Neuronal migration may be impaired during brain development, and impaired molecular motor activity in the adult is one of the hallmarks of neurodegenerative diseases leading to neuronal cell death. The mechanisms that regulate or coordinate kinesin and dynein activity to generate bidirectional transport of the same cargo are of utmost importance. We examined how Ndel1, a cytoplasmic dynein binding protein, may regulate non-vesicular bidirectional transport. Soluble Ndel1 protein, Ndel1-derived peptides or control proteins were mixed with fluorescent beads, injected into the squid giant axon, and the bead movements were recorded using time-lapse microscopy. Automated tracking allowed for extraction and unbiased analysis of a large data set. Beads moved in both directions with a clear bias to the anterograde direction. Velocities were distributed over a broad range and were typically slower than those associated with fast vesicle transport. Ironically, the main effect of Ndel1 and its derived peptides was an enhancement of anterograde motion. We propose that they may function primarily by inhibition of dynein-dependent resistance, which suggests that both dynein and kinesin motors may remain engaged with microtubules during bidirectional transport.

  1. Analysis of Phytomedicines%植物药分析

    Institute of Scientific and Technical Information of China (English)

    余海燕; 吴香玉; 张利民; 唐惠儒

    2012-01-01

    As widely used medicines in the world, phytomedicines played important roles in human health. The analysis of herbal medicines is important for the development of new drugs and functional food. Such analysis includes traditional methods, including metabolite extraction, component isolation and structure elucidation, and the hyphenated techniques with the combination of chromatographic and spectroscopic techniques. Here, we review the general procedures of traditional methods and hyphenated techniques for phytomedicine analysis with emphasis on the hyphenated HPLC-DAD-SPE-NMR-MS techniques.%植物药在世界范围内已经得到了广泛使用,对人类的健康发挥着重要作用.植物药分析是新药、保健食品研发的重要途径.目前,植物药分析方法主要包括传统分析法和联用技术分析法.传统分析法的步骤包括植物药成分提取、分离和结构鉴定.联用技术分析法主要是色谱、质谱、核磁共振等技术的联用.该文对植物药分析的方法尤其是联用技术在植物药分析中的应用进行了综述,重点介绍了HPLC-DAD-SPE-NMR-MS联用技术.

  2. Size exclusion and anion exchange high performance liquid chromatography for characterizing metals bound to marine dissolved organic matter

    Energy Technology Data Exchange (ETDEWEB)

    Garcia-Otero, Natalia; Bermejo-Barrera, Pilar [Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, University of Santiago de Compostela, Avenida das Ciencias, s/n, 15782 Santiago de Compostela (Spain); Moreda-Pineiro, Antonio, E-mail: antonio.moreda@usc.es [Department of Analytical Chemistry, Nutrition and Bromatology, Faculty of Chemistry, University of Santiago de Compostela, Avenida das Ciencias, s/n, 15782 Santiago de Compostela (Spain)

    2013-01-14

    Highlights: Black-Right-Pointing-Pointer Fractionation methods for assessing metals bound to marine DOM were developed. Black-Right-Pointing-Pointer SEC and AEC with UV detection and hyphenated with inductively coupled plasma-mass spectrometry were used. Black-Right-Pointing-Pointer SEC-UV showed marine DOM of molecular weights from 16 to 1 kDa. Black-Right-Pointing-Pointer Cobalt, manganese, strontium and zinc are bound to marine DOM. - Abstract: Size exclusion chromatography (SEC) followed by anion exchange chromatography (AEC) hyphenated with inductively coupled plasma-mass spectrometry (ICP-MS) was applied for fractionating metals bound to marine dissolved organic matter (DOM). Surface seawater samples (100 L) were subjected to tangential flow ultrafiltration (10,000 Da cut off) for isolating and pre-concentrating dissolved large molecules. The isolated fraction (retentate) consisted of 1 L, which was further freeze-dried and re-dissolved to 250 mL with ultrapure water. After HI Trap desalting of the re-dissolved retentate, SEC with UV detection showed marine DOM ranging from 6.5 kDa (lower than the permeable volume of the SEC column) to 16 kDa. A further characterization of this fraction by AEC with UV detection revealed the existence of four groups of macromolecules exhibiting retention times of 2.3, 2.8, 4.5 and 14.0 min. AEC hyphenated with ICP-MS showed the presence of strontium and zinc in the first AE fraction isolated from the SEC fraction; while manganese was found to be bound to the second AE fraction. Cobalt was found to be bound to molecules comprising the third AE fraction.

  3. “I WANT TO BE NOTHING”. CHALLENGING NOTIONS OF CULTURE, RACE AND IDENTITY

    Directory of Open Access Journals (Sweden)

    Agata Lubowicka

    2011-01-01

    Full Text Available This article tackles the issue of “hyphenated identities” in Heidi W. Durrow’s novel The girl who fell from the sky (2010, whose main topic is growing up as a girl of mixed race in a dominant black culture. This article examines how Rachel Morse, the main character in the novel, challenges racism and the essentialist notion of identity. Firstly, Stuart Hall and Paul Gilroy’s approaches to that issue are introduced and discussed. Then in relation to their theories an interpretation of Durrow’s

  4. Information meeting CETAMA; Journees d'information CETAMA

    Energy Technology Data Exchange (ETDEWEB)

    Moulin, C.; Denauwer, C.; Schlegel, M.; Moisy, P.; Gouget, B.; Carriere, M.; Baglan, N.; Reiller, P.; Hanssens, A.; Boullis, B.; Leguay, J.J.; Vercouter, T.; Guilbaud, P.; Taran, F.; Bion, L.; Chaix, P.; Madic, C.; Lecomte, M.; Moulin, C.; Lobinski, R.; Fourest, B.; Hagege, A.; Mercier, F.; Billard, I.; Denecke, M.; Neu, M.; Bernhard, G.; Duffield, J.; Gilbin, R.; Grenthe, I.; Hummel, W.; Turq, P.; Van Der Lee, J

    2004-07-01

    This seminar devoted to the speciation was presented in four main sessions: analytical speciation (actinides and lanthanides speciation, methodology developments, the XPS contribution of hyphenated CE-IPS/MS in metal/protein interaction, spectroscopy...), the applications to the biological and environmental systems (plutonium and neptunium speciation, uranium in plants, radionuclides speciation and interaction with living organisms...), the data bases (advances in chemical thermodynamic database, theoretical chemistry calculation, discovery of powerful uranyl ligands, simulation...) and projects bound to databases and analytical speciation ( BASSIST-GT32, Actinet network, EUROSPART, Gdr Paris, Common Thermodynamic Database Project, ToxNuc-E). (A.L.B.)

  5. Occurrence, biological activities and {sup 13}C NMR data of amides from Piper (Piperaceae)

    Energy Technology Data Exchange (ETDEWEB)

    Nascimento, Jeferson C. do; Paula, Vanderlucia F. de [Universidade Estadual do Sudoeste da Bahia, Jequie, BA (Brazil). Dept. de Quimica e Exatas; David, Jorge M. [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Inst. de Quimica; David, Juceni P., E-mail: jmdavid@ufba.br [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Fac. de Farmacia

    2012-07-01

    This manuscript describes an update review with up to 285 references concerning the occurrence of amides from a variety of species of the genus Piper (Piperaceae). Besides addressing occurrence, this review also describes the biological activities attributed to extracts and pure compounds, a compiled {sup 13}C NMR data set, the main correlations between structural and NMR spectroscopic data of these compounds, and employment of hyphened techniques such as LC-MS, GC-MS and NMR for analysis of amides from biological samples and crude Piper extracts. (author)

  6. 砷形态分析技术研究进展%ADVANCES ON THE ANALYTICAL TECHNIQUE OF ARSENIC SPECIATION

    Institute of Scientific and Technical Information of China (English)

    田靖; 陈昌云

    2011-01-01

    The research advance of separation, detection and hyphenated techniques on arsenic speciation analysis in recent years was summarized. The main issues to be concerned about arsenic speciation analysis in future were put forward.%总结了近年来砷形态分析的分离、检测以及联用技术的研究进展,提出了今后在砷形态分析工作中应关注的主要问题.

  7. 紫外可见分光光度技术的应用进展%Recent Progress of Application of UV-Vis Spectrophotometric Technique

    Institute of Scientific and Technical Information of China (English)

    王海军; 宁新霞

    2012-01-01

    介绍了近几年来紫外可见分光光度技术在仪器部件、多组分体系的测定,新技术应用进展以及与其他技术联用等方面的情况(引用文献33篇)。%An introduction on the recent progress of application of UVVis spectrophotometric technique was presented covering mainly the last several years, relating especially to parts of instrument, determination of multi- component systems, application of new technology and it's hyphenation with other technologies (33 ref. cited).

  8. 花样跑鞋百变秘笈

    Institute of Scientific and Technical Information of China (English)

    凹凹; 花花(设计); 黄剑锋(摄影); JOJO(化妆); Natasha(模特)

    2013-01-01

    Natasha碎花连体裙裤/E hyphen world gallery亮黄色功能跑步鞋/PUMA花花条纹蕾丝连身裙,earthmusic&ecology高帮印花帆布鞋/converse亮粉色短袜/tutuanna PART3 NIKE CLASSIC CORTEZ NYLON 此款鞋履可以说是跑鞋界的元老之物,薄荷绿配色与荧光黄运动衫呼应整身色彩,对热爱运动风的女孩而言势必是个不错的选择。

  9. Method optimization and quality assurance in speciation analysis using high performance liquid chromatography with detection by inductively coupled plasma mass spectrometry

    DEFF Research Database (Denmark)

    Larsen, Erik Huusfeldt

    1998-01-01

    Achievement of optimum selectivity, sensitivity and robustness in speciation analysis using high performance liquid chromatography (HPLC) with inductively coupled mass spectrometry (ICP-MS) detection requires that each instrumental component is selected and optimized with a view to the ideal...... operating characteristics of the entire hyphenated system. An isocratic HPLC system, which employs an aqueous mobile phase with organic buffer constituents, is well suited for introduction into the ICP-MS because of the stability of the detector response and high degree of analyte sensitivity attained...

  10. ISIDORE, a probe for in situ trace metal speciation based on Donnan membrane technique with related electrochemical detection part 1: Equilibrium measurements.

    Science.gov (United States)

    Parat, Corinne; Pinheiro, J P

    2015-10-01

    This work presents the development of a new probe (ISIDORE probe) based on the hyphenation of a Donnan Membrane Technique device (DMT) to a screen-printed electrode through a flow-cell to determine the free zinc, cadmium and lead ion concentration in natural samples, such as a freshwater river. The probe displays many advantages namely: (i) the detection can be performed on-site, which avoids all problems inherent to sampling, transport and storage; (ii) the low volume of the acceptor solution implies shorter equilibration times; (ii) the electrochemical detection system allows monitoring the free ion concentration in the acceptor solution without sampling. PMID:26481984

  11. Historiography and Historicality

    OpenAIRE

    Garba, Ismail Bala

    2013-01-01

    Note portant sur l’auteur Ranajit Guha, History at the Limit of World-History, New York: Columbia University Press, 2002,128 pp. ISBN 0-231-12418-X, Hardback Ranajit Guha’s History at the Limit of World-History fuses, as it were, both practice and theory by conceptualising “world history” (without the hyphen) in such a way as to see it critically as a problem of whether it is possible to achieve any level of speciality in an enormous field of that name. What was once regarded as world history...

  12. Direct coupling of a flow-flow electromembrane extraction probe to LC-MS

    DEFF Research Database (Denmark)

    Fuchs, David; Gabel-Jensen, Charlotte; Jensen, Henrik;

    2016-01-01

    A fully integrated and automated electromembrane extraction LC-MS (EME-LC-MS) system has been developed and characterized. Hyphenation of a flow-flow EME probe to LC-MS was accomplished by using an in-built 10-port switching valve of the LC-MS system. The 10-port switching valve decoupled the high...... pressure of the UHPLC-system from the low pressure required for operation of the EME-probe by automated switching between a sample extraction/analysis and a sample load position. In the sample load position the extracted analytes were loaded into a HPLC sample loop. By switching the valve to the sample...

  13. Grammatically Correct The Essential Guide to Spelling, Style, Usage, Grammar, and Punctuation

    CERN Document Server

    Stilman, Anne

    2010-01-01

    How does good writing stand out? If its purpose is to convey facts, findings, or instructions, it need be read only once for its content to be clear. If its purpose is to entertain or to provoke thought, it makes readers want to come back for more. Revised and updated, this guide covers four essential aspects of good writing:Individual words - spelling variations, hyphenation, frequently confused homonyms, frequently misused words and phrases, irregular plurals and negatives, and uses of capitalization and type style to add special meaningsPunctuation - the role of each mark in achieving clar

  14. Determination of cadmium and lead species and phytochelatins in pea (Pisum sativum) by HPLC-ICP-MS and HPLC-ESI-MSn.

    Science.gov (United States)

    Barałkiewicz, Danuta; Kózka, Małgorzata; Piechalak, Aneta; Tomaszewska, Barbara; Sobczak, Paweł

    2009-07-15

    An analytical approach based on hyphenated techniques was used for studying the speciation of cadmium and lead in Pisum sativum. Proper preservation conditions were employed to avoid the oxidation of -SH groups and corresponding decomposition of metal-binding complexes. SEC column was washed with 5 mM beta-mercaptoethanol and then samples were analysed using ICP-MS as a detector. Results showed that cadmium is the inhibitor of lead uptake. HPLC-ESI-MS(n) assays revealed fragmentation pathways of phytochelatins.

  15. Methyl mercury in nail clippings in relation to fish consumption analysis with gas chromatography coupled to inductively coupled plasma mass spectrometry: a first orientation.

    Science.gov (United States)

    Krystek, Petra; Favaro, Paulo; Bode, Peter; Ritsema, Rob

    2012-08-15

    For the identification of human exposure to one of the most toxic compounds, which is methyl mercury (MeHg(+)), fingernail clippings were selected as the matrix of interest. Within this pilot study, six samples from different origins and from people with different food consumption patterns were chosen. Species-analysis of MeHg(+) was performed according to the following procedure: dissolution of the sample material in tetramethylammonium hydroxide (TMAH), derivatisation of MeHg(+) with sodium tetraethylborate (NaBEt(4)), extraction into iso-octane and measurement with gas chromatography hyphenated to inductively coupled plasma mass spectrometry (GC-ICPMS) for the quantification MeHg(+).

  16. A dupla face de Janus da China

    Directory of Open Access Journals (Sweden)

    Henrique Rattner

    2010-06-01

    Full Text Available Na mitologia romana, Janus é o rei mais antigo do Latium. Por ter acolhido a Saturno, expulso do Olimpo, este lhe brindou com uma visão em que tanto o futuro quanto o passado estivessem presentes, ficando assim conhecido como dono de duas faces. Essa duplicidade de personagem aplica-se perfeitamente ao papel da política chinesa, neste início de século XXI.

  17. NRC [Nuclear Regulatory Commission] editorial style guide

    International Nuclear Information System (INIS)

    Editorial style refers to the choices that writers, editors, and secretaries make to eliminate inconsistencies in their documents. These choices apply to the recurrent features of a document such as abbreviations, capitalization, compound words, numbers, symbols, and punctuation, as well as to references and footnotes. Making these choices is sometimes difficult because usage changes as the language evolves. Consider the use of hyphens, for example. Do we write non-power reactor or nonpower reactor? Is it on-site incident or onsite incident? Although usage is moving away from the use of hyphens with prefixes, the authorities who compile style guides do not always agree about which choice to use at a given time. Moreover, each discipline -- law, physics, mathematics -- has specific standards that apply to the publications for that discipline. Even in an area as seemingly certain as spelling, overlapping usage exists. Reputable dictionaries show both ''align'' and ''aline'' as correct spellings. Likewise, ''disc, disk, and diskette'' currently coexist as equally valid choices

  18. 双周至潮事件无码解密

    Institute of Scientific and Technical Information of China (English)

    2015-01-01

    演绎趣味更浓的自在摩登 留学巴黎的E hyphen girl,将自在、趣味、摩登与巴黎艺术与时尚完美结合,不论打球、上课,还是逛展览,都能演绎出自己独特的穿搭法则。E hyphen world gallery 2015年春季系列便是留学巴黎的摩登女性的趣味艺术之旅,设计师将年轻女性的个性诉求与别样心机融入巴黎时尚之中,开启舂日女生自我发现的新鲜之旅。网球图案、波普水果印花、条纹格纹等元素让这一季增添不少运动与艺术气患,春意盎然的明快色调让春目的活力与张扬尽情释放。

  19. Comparison of high-performance liquid chromatography and supercritical fluid chromatography using evaporative light scattering detection for the determination of plasticizers in medical devices.

    Science.gov (United States)

    Lecoeur, Marie; Decaudin, Bertrand; Guillotin, Yoann; Sautou, Valérie; Vaccher, Claude

    2015-10-23

    Recently, interest in supercritical fluid chromatography (SFC) has increased due to its high throughput and the development of new system improving chromatographic performances. However, most papers dealt with fundamental studies and chiral applications and only few works described validation process of SFC method. Likewise, evaporative light scattering detection (ELSD) has been widely employed in liquid chromatography but only a few recent works presented its quantitative performances hyphenated with SFC apparatus. The present paper discusses about the quantitative performances of SFC-ELSD compared to HPLC-ELSD, for the determination of plasticizers (ATBC, DEHA, DEHT and TOTM) in PVC tubing used as medical devices. After the development of HPLC-ELSD, both methods were evaluated based on the total error approach using accuracy profile. The results show that HPLC-ELSD was more precise than SFC-ELSD but lower limits of quantitation were obtained by SFC. Hence, HPLC was validated in the ± 10% acceptance limits whereas SFC lacks of accuracy to quantify plasticizers. Finally, both methods were used to determine the composition of plasticized-PVC medical devices. Results demonstrated that SFC and HPLC both hyphenated with ELSD provided similar results.

  20. Elemental ratios for characterization of quantum-dots populations in complex mixtures by asymmetrical flow field-flow fractionation on-line coupled to fluorescence and inductively coupled plasma mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Menendez-Miranda, Mario; Fernandez-Arguelles, Maria T.; Costa-Fernandez, Jose M., E-mail: jcostafe@uniovi.es; Encinar, Jorge Ruiz; Sanz-Medel, Alfredo, E-mail: asm@uniovi.es

    2014-08-11

    Highlights: • The hyphenated system allows unequivocal identification of nanoparticle populations. • AF4 separation permitted detection of unexpected nanosized species in a sample. • ICP-QQQ provides elemental ratios with adequate accuracy in every nanoparticle. • Purity and chemical composition of different quantum dot samples were assessed. - Abstract: Separation and identification of nanoparticles of different composition, with similar particle diameter, coexisting in heterogeneous suspensions of polymer-coated CdSe/ZnS quantum dots (QDs) have been thoroughly assessed by asymmetric flow field-flow fractionation (AF4) coupled on-line to fluorescence and inductively coupled plasma mass spectrometry (ICPMS) detectors. Chemical characterization of any previously on-line separated nanosized species was achieved by the measurement of the elemental molar ratios of every element involved in the synthesis of the QDs, using inorganic standards and external calibration by flow injection analysis (FIA). Such elemental molar ratios, strongly limited so far to pure single nanoparticles suspensions, have been achieved with adequate accuracy by coupling for the first time an ICP-QQQ instrument to an AF4 system. This hyphenation turned out to be instrumental to assess the chemical composition of the different populations of nanoparticles coexisting in the relatively complex mixtures, due to its capabilities to detect the hardly detectable elements involved in the synthesis. Interestingly such information, complementary to that obtained by fluorescence, was very valuable to detect and identify unexpected nanosized species, present at significant level, produced during QDs synthesis and hardly detectable by standard approaches.

  1. Tandem mass spectrometry in metallomics and the involving role of ICP-MS detection: a review.

    Science.gov (United States)

    Vogiatzis, C G; Zachariadis, G A

    2014-03-28

    Metallomics is a relatively new branch of omics with a growing interest. The study of metallomes is becoming more focused in certain metabolites and the screening of various categories of analytes using a robust analytical methodology is more than appealing. In this context, when dealing with the challenge of identifying a certain species or specify a particular molecular structure, tandem mass spectrometry (MS/MS) is a reliable tool. Moreover, MS/MS instrumentation is recommended in hyphenated chromatographic techniques with MS detection such as LC-MS, where primary molecular species suffer minor fragmentation (soft-ionization techniques). ICP-MS is widely used in metallomics with its main advantages being the provided high sensitivity and selectivity. Usually, analyzes utilize ICP-MS as the main detection. Its role in proteomics is significant as an alternating choice for protein and peptide quantifications. In this review, we discuss modern trends and applications of MS/MS in the important and growing field of metallomics. These reports concern the identification, characterization and determination of various metal species such as metalloproteins, metallo-DNA adducts, metal-labeled molecules and other metal binding biomolecules. Such assays also present new and interesting hyphenated instrumentation and novel sophisticated apparatus. In addition, we designate the role of ICP-MS in the mentioned contributions and in the same scope we highlight some general analytical strategies.

  2. [Analysis of irregularities in writing English and Serbian professional papers].

    Science.gov (United States)

    Kernican, Leotina; Mićić, Sofija

    2008-01-01

    There are many peculiarities and indecisions in the English and Serbian language. One of the crucial is doubtless a translation from Serbian into English. On the other hand, by analysing professional papers of English native speakers, a tendency of greater conciseness is shown. Thus a better knowledge of etymological structure and modern formal style in both languages is essential. Accordingly, it is of utmost importance to pay a special attention to appropriate collocations, text summarizing and various possible mistakes ranging from wrong spelling and improper use of some abbreviations of conventional titles to incorrect capitalization, hyphenated words, etc. Language is certainly a vivid unique style of each personality, even in professional formal writing, but, by using it, we naturally enrich the expression and quality of the language as a whole. PMID:18720760

  3. Microfluidic chip for stacking, separation and extraction of multiple DNA fragments.

    Science.gov (United States)

    Wu, Ruige; Seah, Y P; Wang, Zhiping

    2016-03-11

    A disposable integrated microfluidic device was developed for rapid sample stacking, separation and extraction of multiple DNA fragments from a relatively large amount of sample. Isotachophoresis hyphenated gel electrophoresis (ITP-GE) was used to pre-concentrate and separate DNA fragments, followed by extraction of pure DNA fragments with electroelution on-chip. DNA fragments of 200bp, 500bp and 1kbp were successfully separated and collected in the extraction chamber within 25min. The extraction efficiency obtained from the chip was 49.9%, 52.1% and 53.7% for 200bp, 500bp and 1kbp DNA fragments, respectively. The extracted DNA fragments exhibited compatibility with downstream enzymatic reactions, for example PCR. The chip was also used to extract DNA fragments with specific size range from sheared genomic DNA and demonstrated similar performance to that using traditional gel cutting method. The whole assay can finish in 32min, 6 times faster than traditional method.

  4. Recent trends in rapid dereplication of natural product extracts:an update

    Institute of Scientific and Technical Information of China (English)

    Fikre Mammo; Milkyas Endale

    2015-01-01

    Natural products are the prominent sources of drugs to combat various infectious diseases. The rapid progress of multi-resistance and pan-resistant pathogens to various medicines represents today a major challenge. The search for novel natural products requires a quick and efficient approach to distinguish novel compounds from the known ones, a process called dereplication. Dereplication strategy is generic and time-saving, avoids isolation/purification of known compounds, enables an efficient liquid chromatography peak annotation of most of the studied compounds and can be well adapted for plant chemotaxonomy, phytochemical screening and metabolite profiling. In this review, recent developments of hyphenated techniques towards dereplication of active compounds, chemotaxonomy, metabolite profiling and rapid detection of novel compounds in medicinal plant extracts are presented.

  5. Lignin profiling in extracted xylans by size-exclusion chromatography.

    Science.gov (United States)

    Hutterer, Christian; Schild, Gabriele; Kliba, Gerhard; Potthast, Antje

    2016-10-20

    Utilization of the polymeric parts of lignocellulose is expected to gain increasing importance in future biorefinery scenarios. In that respect, a particular focus is placed on hemicelluloses from different wood species gained from an industrially feasible upgrading step in the production of dissolving pulps from paper pulps. During alkaline post-extractions for hemicellulose removal, residual lignins are extracted as well. They are either covalently linked to the extracted hardwood xylans or simply co-dissolved in the alkaline lye. In order to better describe the lignin in xylan containing lyes, a method for lignin profiling was set up by hyphenating size-exclusion chromatography of xylans with UV detection which facilitates visualization of the residual lignin distribution. Simultaneous lignin quantification was achieved with lignin standards prepared from Kraft cooking liquors. The setup presented may serve as advanced characterization for novel xylan products. PMID:27474629

  6. Separation and identification of phenolic compounds of extra virgin olive oil from Olea europaea L. by HPLC-DAD-SPE-NMR/MS. Identification of a new diastereoisomer of the aldehydic form of oleuropein aglycone.

    Science.gov (United States)

    Pérez-Trujillo, Míriam; Gómez-Caravaca, Ana María; Segura-Carretero, Antonio; Fernández-Gutiérrez, Alberto; Parella, Teodor

    2010-08-25

    The phenolic fraction of a monovarietal extra virgin olive oil (EVOO) from Olea europaea L. var. Cornezuelo was studied by the hyphenated HPLC-DAD-SPE-NMR/MS techniques. This survey led to the identification of 25 main compounds. One was identified as a new diastereoisomer of the aldehydic form of oleuropein aglycone (AOA) and characterized by 1D and 2D NMR techniques. The relative configuration of this new AOA was determined as 5R*,8S*,9S* on the basis of the results obtained from the combination of NOE experiments and Monte Carlo conformational search calculations. Assuming, as for the described diastereoisomers, that the new AOA comes from the natural oleuropein aglycone (OA), the absolute configuration was proposed as 5S,8R,9R.

  7. Secoiridoids in olive seed: characterization of nuzhenide and 11-methyl oleosides by liquid chromatography with diode array and mass spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Silva, S.; Gomes, L.; Leitao, F.; Bronze, M.; Coelho, A. V.; Vilas Boas, L.

    2010-07-01

    The seed extracts of olive tree cultivars were analyzed by reverse phase HPLC with diode array detection and mass spectrometry. HPLC hyphenation with mass spectrometry (Ei source) in both polarity modes enabled the identification in olive seeds of nuzhenide and nuzhenide 11-methyl oleoside, among other 11-methyl oleosides, by means of MSn. The methods used allowed us to obtain olive seed profiles of phenolic components and to conclude that they are mainly secoiridoids. The quantification of detected phenolic secoiridoids was also achieved using ultraviolet detection ({lambda}= 240 nm) which enabled comparison of the samples. Nuzhenide and nuzhenide 11-methyl oleoside were the major components detected in olive seeds of all the cultivars studied, but variations in individual components of olive seeds were verified among the cultivars. The results also support the existence of di and tri(11-methyl oleosides) of nuzhenide. (Author)

  8. Novel applications of high performance ion chromatography-inductively coupled plasma mass spectrometry (HPIC-ICP-MS)

    CERN Document Server

    Hann, S

    2001-01-01

    This work demonstrates the development of highly sensitive and selective analytical methods, which make use of the hyphenation of high performance ion chromatography (HPIC) to inductively coupled plasma sector field mass spectrometry (ICP-SFMS). On-line coupling a chromatographic separation method with an elemental detection method provides two advantages: (1) the components of a possibly interfering matrix can be separated allowing accurate and precise ultra trace analysis of the element of interest and (2) elemental species of an element can be separated and quantified. In this work, matrix separation methods for interference free determination of 232Th, 234U, 235U and 238U in geological matrices were developed and employed. Furthermore HPIC-ICP-SFMS was applied for ultra trace analysis of Pd in environmental and geological matrices. The usefulness of HPIC-ICP-SFMS for speciation studies was demonstrated by investigating the interaction of an anti-cancer drug (cisplatin) with guanosine monophosphates.

  9. Analytical developments for screening of lanthanides/ligands interactions

    International Nuclear Information System (INIS)

    This work investigates the potential of hyphenated capillary electrophoresis and inductively coupled mass spectrometry to classify different ligands according to their europium binding affinity in a hydro-organic medium. On the one hand, this method enables to evaluate the affinity of phosphorus-containing ligands in less than two hours and using less than 15 ng of ligand. On the other hand, complexation constants could be determined. The results are in excellent agreement with the values obtained by spectrophotometric titrations.Moreover, a library of copolymers for solid/liquid extraction of europium is investigated. The extraction protocol enables to classify copolymers according to their europium affinity in a hydro-organic medium. This screening requires 60 mg of copolymers. For the most promising recognition properties and selectivity La3+/Eu3+/Lu3+ are evaluated. (author)

  10. Determination of Kinetic Parameters within a Single Nonisothermal On-Flow Experiment by Nanoliter NMR Spectroscopy.

    Science.gov (United States)

    Gomez, M Victoria; Rodriguez, Antonio M; de la Hoz, Antonio; Jimenez-Marquez, Francisco; Fratila, Raluca M; Barneveld, Peter A; Velders, Aldrik H

    2015-10-20

    Conventional methods to determine the kinetic parameters for a certain reaction require multiple, separate isothermal experiments, resulting in time- and material-consuming processes. Here, an approach to determine the kinetic information within a single nonisothermal on-flow experiment is presented, consuming less than 10 μmol of reagents and having a total measuring time of typically 10 min. This approach makes use of a microfluidic NMR chip hyphenated to a continuous-flow microreactor and is based on the capabilities of the NMR chip to analyze subnanomole quantities of material in the 25 nL detection volume. Importantly, useful data are acquired from the microreactor platform in specific isothermal and nonisothermal frames. A model fitting the experimental data enables rapid determination of kinetic parameters, as demonstrated for a library of isoxazole and pyrazole derivatives. PMID:26383715

  11. Rapid prototyping of microfluidic chips for dead-volume-free MS coupling.

    Science.gov (United States)

    Dietze, Claudia; Scholl, Tobias; Ohla, Stefan; Appun, Johannes; Schneider, Christoph; Belder, Detlev

    2015-11-01

    A fast and straightforward method to prototype microfluidic chip systems for dead-volume-free hyphenation to electrospray-ionisation mass spectrometry is presented. The developed approach based on liquid-phase lithography provides an inexpensive and reliable access to microfluidic chips for MS coupling which can be manufactured in any laboratory with low technical demands. The rapid prototyping approach enables the seamless integration of capillaries serving as electrospray emitters with negligible dead volume. The high versatility of the presented prototyping method and the applicability of a variety of chip-based devices in different fields of lab-on-a-chip technology are established for analytical separations by means of chip-electrochromatography-MS and for continuous-flow synthesis using microreactor technology with MS detection. PMID:26391402

  12. Pressurized liquid extraction and HPLC quantification of folic acid in fortified wheat flours.

    Science.gov (United States)

    Araújo, Michel Mozeika; Marchioni, Eric; Villavicencio, Anna Lucia Casañas Haasis; Zhao, Minjie; Zimmermann, Pierre; El-Khoury, Etienne; Bergaentzle, Martine

    2012-08-01

    A pressurized liquid extraction (PLE) method using phosphate buffer as solvent was applied for folic acid (FA) extraction from fortified wheat flours and was compared to a standard solid-liquid extraction (SLE) method. Extracted FA was quantified by reverse phase high-performance liquid chromatography (RP-HPLC) hyphenated with a phenyl column and an absorption photometric detector (λ = 280 nm). Detection and quantification limits were 0.12 and 0.4 ng, respectively, corresponding to 0.06 and 0.2 μg g(-1) of analyzed wheat flour. Equivalent FA contents were found by both extraction methods, but a single PLE allowed a total recovery of FA content, whereas at least three successive SLEs were needed to achieve a total recovery of FA. The obtained results indicated that PLE is a rapid and efficient technique for FA extraction from fortified wheat flour.

  13. Mental illness in the nursing workplace: a collective autoethnography.

    Science.gov (United States)

    Kidd, Jacquie Dianne; Finlayson, Mary P

    2010-01-01

    Many nurses are burned out, exhausted and have a high intent to leave their jobs. These factors, when experienced over a period of time, are consistent with the development of mental illness. This study takes a collective autoethnographical approach to mental illness in the nursing workplace by focusing on the stories of nurses who have experienced mental illness in clinical practice. It highlights three ways in which nursing and mental illness are connected; the nurse who is vulnerable to mental illness prior to entering the profession, the nurse who develops mental illness that is independent of her work but is nevertheless impacted by it, and the nurse who develops mental illness as a result of her work and/or role. This paper explores the hyphenated lives and bullying these nurses experience, and recommends strategies that the profession, employing organisations, and individuals can adopt to reduce nurses' progression from stress to distress and mental illness. PMID:21254820

  14. The Expanding Role of NMR in Drug Discovery and Development

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    @@ The role of NMR in the pharmaceutical industry has changed dramatically over the last decade. Once thought of as an analytical technique used primarily to support synthetic chemistry, NMR now has an important role in the investigation of biochemical changes involved in clinical diseases and drug toxicity. It is also used extensively to elucidate the structures of drug metabolites. Data obtained using LC NMR MS and 19F NMR will be used to illustrate the utility of hyphenated methods in identifying xenobiotic metabolites as part of a drug development program. The application of NMR to the study of potential drug toxicity will also be described using the cationic, amphiphilic drugs chloroquine and amiodarone. These drugs are known to induce phospholipidosis characterized by lysosomal lamellar bodies and drug accumulation. Using a metabonomic approach, NMR spectroscopy of urine allowed the identification of a combination of urinary biomarkers of phospholipidosis.

  15. Recent applications of liquid chromatography-mass spectrometry in natural products bioanalysis.

    Science.gov (United States)

    Xing, Jie; Xie, Chunfeng; Lou, Hongxiang

    2007-06-28

    Natural flavonoids, alkaloids, saponins and sesquiterpenoids have been extensively investigated because of their biological and physiological significances, as well as their promising clinical uses. It is necessary to monitor them or their metabolites in biological fluids for both pre-clinical studies and routine clinical uses. The successful hyphenation of LC and MS, which was thought as "the bird wants to marry with fish", has been conducted widely in biological samples analysis. This present paper reviewed the feasibility of LC-MS techniques in the identification and quantification of natural products (flavonoids, alkaloids, saponins and sesquiterpenoids) in biological fluids, dealing with sample preparation, LC techniques, suitability of different MS techniques. Perspective of LC-MS was also discussed to show the potential of this technology. The citations cover the period 2002-2006. We conclude that LC-MS is an extremely powerful tool for the analysis of natural products in biological samples. PMID:17317073

  16. Targeted natural product isolation guided by HPLC-SPE-NMR: Constituents of Hubertia species

    DEFF Research Database (Denmark)

    Sprogoe, K.; Staek, D.; Jager, A.K.;

    2007-01-01

    The hyphenated technique, high-performance liquid chromatography-solid-phase extraction-nuclear magnetic resonance spectroscopy (HPLC-SPE-NMR), has been applied for rapid identification of novel natural products in crude extracts of Hubertia ambavilla and Hubertia tomentosa. The technique allowed...... full or partial identification of all major extract constituents and demonstrated the presence of unusual quinic acid derivatives containing the (1-hydroxy-4-oxocyclohexa-2,5-dienyl)acetyl residue that exhibit strongly coupled ABXY patterns, the parameters of which were obtained by spin simulations....... Using homo- and heteronuclear 2D NMR data acquired in the HPLC-SPE-NMR mode, complete structure determination of three new natural products, i.e., 3,5-di-O-caffeoyl-4-O-[(1-hydroxy-4-oxocyclohexa-2,5-dienyl)acetyl]quini c acid (1), its 2-hydroxy derivative (2), and 3,5-di-O-caffeoyl-4-O-[(4...

  17. Advanced analytical techniques for the extraction and characterization of plant-derived essential oils by gas chromatography with mass spectrometry.

    Science.gov (United States)

    Waseem, Rabia; Low, Kah Hin

    2015-02-01

    In recent years, essential oils have received a growing interest because of the positive health effects of their novel characteristics such as antibacterial, antifungal, and antioxidant activities. For the extraction of plant-derived essential oils, there is the need of advanced analytical techniques and innovative methodologies. An exhaustive study of hydrodistillation, supercritical fluid extraction, ultrasound- and microwave-assisted extraction, solid-phase microextraction, pressurized liquid extraction, pressurized hot water extraction, liquid-liquid extraction, liquid-phase microextraction, matrix solid-phase dispersion, and gas chromatography (one- and two-dimensional) hyphenated with mass spectrometry for the extraction through various plant species and analysis of essential oils has been provided in this review. Essential oils are composed of mainly terpenes and terpenoids with low-molecular-weight aromatic and aliphatic constituents that are particularly important for public health.

  18. 毛细管电泳-电致化学发光联用技术应用进展%Recent Progress of Application of CE-ECL

    Institute of Scientific and Technical Information of China (English)

    胡月芳; 李建平; 刘蓉; 郝再彬

    2011-01-01

    A review on the application of capillary electrophoresis hyphenated with electrochemiluminescence (CE-ECL) was presented, relating especially to its principle and application to analysis of pharmaceutical, biological, environmental, food and agricultural samples during the years from 1983-2010. (66 ref. Cited).%介绍了毛细管电泳-电致化学发光联用技术(CE-ECL)的检测原理,重点评述了1983-2010年间CE-ECL在药物制品、生物样品、环境和食品、农产品分析中的应用(引用文献66篇)。

  19. DART-MS:A New Research Tool for Herbal Medicine Analysis

    Institute of Scientific and Technical Information of China (English)

    Yao Shen; Wan-Ying Wu; De-An Guo

    2016-01-01

    Direct analysis in real time (DART) possesses the merits of analyzing sample in its native status with minimal or even no sample pretreatment. In this review, we summarized the recent applications of DART in the field of herbal medicine analysis such as compound detection, species identification, metabolites profiling and initial quantification. DART with the characters of hyper-rapid, easy-hyphenated offers a new research tool for herbal medicines to complete the experimental process in a very simple but still reliable way. It is anticipated that more wide and deep applications of DART in herbal medicine analysis, as rapid quantification, high-throughput active compounds screening, rapid species identification, and fast illegal additives screening will be promising and foreseeable in the near future.

  20. 汞结合金属硫蛋白的色谱-质谱表征方法%Characterization of Mercurial-bound Metallothioneins in Tissues of Rat Kidney by Chromatography Coupled With ICP-MS and ESI-MS

    Institute of Scientific and Technical Information of China (English)

    黄志勇; 沈金灿; 庄峙厦; 王小如; 黎先春

    2004-01-01

    Mercurial-bound metallothioneins (MTs) induced in kidney of rat after oral intake of HgCl2 were characterized with the developed hyphenated techniques including reverse phase chromatography (RPC) coupled with inductively coupled plasma mass spectrometry (ICPMS) and electrospray ionization mass spectrometry(ESIMS). After being purified with size-exclusion column (Sephadex G-75) and dialysis (M<1000 Da), the extracts was separated with a narrow-bore reverse phase column and eluted by increasing methanol at gradient mode. The MT polymorphism with different binding-metal (including Hg, Cu and Zn) species was interpreted by the measured masses at the vicinity of apexes in total ion current (TIC) of ESIMS and the reference data of apo-MTs reported.The results indicated that many Hg-binding MT species existed in the polluted rat kidney.

  1. 膜分离在中药制药中的应用进展%Application progress on the production of traditional Chinese medicine using membrane separation

    Institute of Scientific and Technical Information of China (English)

    樊君; 代宏哲; 高续春

    2011-01-01

    This article reviews recent developments of membrane technology such as microfiltration, ultra-filtration, nanofiltration, reverse osmosis, molecularly imprinted membrane, membrane distillation and hyphenated techniques in the membrane separation. Then, the field and the status quo of membrane separation in the production of traditional Chinese medicine are given and the applications of membrane separation in future are prospected.%对膜分离技术在中药生产过程中的应用领域以及常用的微滤、超滤、纳滤、反渗透、分子印迹膜、膜蒸馏和膜集成联用技术等的应用现状进行了综述,并对膜分离技术的应用前景进行了展望.

  2. Study on Retention in Liquid Chromatography%关于液相色谱保留的研究

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    After joining the faculty at Toyohashi University of Technology (TUT) in 1978, the author has found two areas in separation sciences where microcolumn liquid chromatography (micro-LC) can be beneficial. One is the hyphenated techniques between many spectroscopic methods such as mass (MS), infrared (FT-IR) and atomic emission (ICP), and micro-LC. The other one is rather difficult, but basic and theoretical approach which deals with retention mechanism in LC. The latter project has especially been giving him a lot of scientific funs and honors in the last 20 years. On the occasion of being awarded by The Society for Chromatographic Sciences the author would like to summarize his contributions to this topic which asks us "What Is Chromatographic Retention".

  3. The master plot in the audiovisual narrative. The western case.

    Directory of Open Access Journals (Sweden)

    José Félix GONZÁLEZ SÁNCHEZ

    2015-05-01

    Full Text Available A plot provides us the story that it offers a hyphen and later a film. Plots are limited, however possibilities, argument them that these offer music infinite. At the same time, we can say that all cultures avail themselves of some plots and similar arguments to structure their mythical stories. In addition, United States is the modern nation where better a dialectic relation between the myth and story keeps. At this nation, the significance of the event has been shown and you have gotten free through the myth. We will see through this article how the western is the kind of American cinema what else and better answer for the folkloric traditional story to the cánones, because your plots have been taken directly of the classical legends.

  4. Ribeiro ou Miranda-Ribeiro? Nota biográfica sobre Alípio de Miranda Ribeiro (1874-1939 Ribeiro or Miranda-Ribeiro? A biographical note on Alípio de Miranda Ribeiro (1874-1939

    Directory of Open Access Journals (Sweden)

    José P Pombal Jr

    2002-09-01

    Full Text Available Alípio de Miranda Ribeiro was one of the foremost Brazilian naturalists of his era and published extensively on all vertebrate groups. His son, Paulo de Miranda Ribeiro (1901-1965, was an ichthyologist, and, as his father, worked at the Museu Nacional, in Rio de Janeiro. Brazil. Although the papers of Alípio and Paulo de Miranda Ribeiro are commonly cited, two distinct forms are found: Ribeiro and Miranda-Ribeiro. The use a hyphen between Miranda and Ribeiro (spo-radically, and verified names of ancestor and descendants suggest that the better form for citation is Miranda-Ribeiro. A short biographical note on Alípio de Miranda-Ribeiro is provided.

  5. 汞结合金属硫蛋白的色谱-质谱表征方法

    Institute of Scientific and Technical Information of China (English)

    黄志勇; 沈金灿; 庄峙厦; 王小如; 黎先春

    2004-01-01

    Mercurial-bound metallothioneins (MTs) induced in kidney of rat after oral intake of HgCl2 were characterized with the developed hyphenated techniques including reverse phase chromatography (RPC) coupled with inductively coupled plasma mass spectrometry (ICPMS) and electrospray ionization mass spectrometry(ESIMS). After being purified with size-exclusion column (Sephadex G-75) and dialysis (M<1000 Da), the extracts was separated with a narrow-bore reverse phase column and eluted by increasing methanol at gradient mode. The MT polymorphism with different binding-metal (including Hg, Cu and Zn) species was interpreted by the measured masses at the vicinity of apexes in total ion current (TIC) of ESIMS and the reference data of apo-MTs reported.The results indicated that many Hg-binding MT species existed in the polluted rat kidney.

  6. 高铁氧化技术在环境污染治理中的应用及研究进展%The Application and Advances of Potassium Ferrate in Removal of Pollutents

    Institute of Scientific and Technical Information of China (English)

    马超

    2012-01-01

    Potassium ferrate technology has been paied more and more attention with advantage of itself.The article introduces the preparation of potassium ferrate and the mechanism of pollutants processing,discusses the main influence factors in the pollutants processing.It states the advances in hypHenated techniques.by combination of potassium ferrate and other treatment techniques.%高铁氧化技术在环境污染治理中因其自身所具有的优势而得到越来越多的重视,文章介绍了高铁盐在污染物处理的作用机理,讨论了高铁盐在处理污染物过程中主要影响因素。简述高铁氧化技术与其他处理技术协同作用的研究进展。

  7. Application of LC-MS/MS for quantitative analysis of glucocorticoids and stimulants in biological fluids

    Institute of Scientific and Technical Information of China (English)

    Jamshed Haneef; Mohammad Shaharyar; Asif Husaina; Mohd Rashid; Ravinesh Mishra; Shama Parveen; Niyaz Ahmed; Manoj Pal; Deepak Kumar

    2013-01-01

    Liquid chromatography tandem mass chromatography (LC-MS/MS) is an important hyphenated technique for quantitative analysis of drugs in biological fluids. Because of high sensitivity and selectivity, LC-MS/MS has been used for pharmacokinetic studies, metabolites identification in the plasma and urine. This manuscript gives comprehensive analytical review, focusing on chromatographic separation approaches (column packing materials, column length and mobile phase) as well as different acquisition modes (SIM, MRM) for quantitative analysis of glucocorticoids and stimulants. This review is not meant to be exhaustive but rather to provide a general overview for detection and confirmation of target drugs using LC-MS/MS and thus useful in the doping analysis, toxicological studies as well as in pharmaceutical analysis.

  8. Design and implementation of an automated liquid-phase microextraction-chip system coupled on-line with high performance liquid chromatography

    DEFF Research Database (Denmark)

    Li, Bin; Petersen, Nickolaj J.; Payán, María D Ramos;

    2014-01-01

    An automated liquid-phase microextraction (LPME) device in a chip format has been developed and coupled directly to high performance liquid chromatography (HPLC). A 10-port 2-position switching valve was used to hyphenate the LPME-chip with the HPLC autosampler, and to collect the extracted....... The composition of the supported liquid membrane (SLM) and carrier was optimized in order to achieve reasonable extraction performance of all the five alkaloids. With 1-octanol as SLM solvent and with 25mM sodium octanoate as anionic carrier, extraction recoveries for the different opium alkaloids ranged between...... analytes, which then were delivered to the HPLC column. The LPME-chip-HPLC system was completely automated and controlled by the software of the HPLC instrument. The performance of this system was demonstrated with five alkaloids i.e. morphine, codeine, thebaine, papaverine, and noscapine as model analytes...

  9. Methods for analysis of the distribution and speciation of iron and zinc in the cereal grain

    DEFF Research Database (Denmark)

    Hansen, Thomas Hesselhøj

    certified reference materials. This enabled high-throughput analysis of different grain tissue fractions and the variability in between them.. Moreover two methods for quantitative hyphenated ICP-MS analysis were developed. One enabled quantification of species in a chromatographic separation and the other......-localization and identification of P and S with mineral micronutrients can therefore be a circumstantial evidence for their chemical speciation. The focus of this PhD has therefore been on the analysis of mineral micronutrients as well as S and P. In this PhD, four methods for elemental analysis of the cereal grain have been......, a novel high-throughput micro digestion method was developed, enabling the analysis of total element concentrations in small tissue fractions, such as the embryo of cereal grains. The method is based on small closed bombs that are microwaved and was validated for sample amounts between 1-20 mg using...

  10. Triple aldose reductase/α-glucosidase/radical scavenging high-resolution profiling combined with high-performance liquid chromatography – high-resolution mass spectrometry – solid-phase extraction – nuclear magnetic resonance spectroscopy for identification of antidiabetic constituents in crude

    DEFF Research Database (Denmark)

    Tahtah, Yousof; Kongstad, Kenneth Thermann; Wubshet, Sileshi Gizachew;

    2015-01-01

    high-performance liquid chromatography – high-resolution mass spectrometry – solid-phase extraction – nuclear magnetic resonance spectroscopy. The only α-glucosidase inhibitor was baicalein, whereas main aldose reductase inhibitors in the crude extract were baicalein and skullcapflavone II, and main....../α-glucosidase/radical scavenging high-resolution inhibition profile - allowing proof of concept with Radix Scutellariae crude extract as a polypharmacological herbal drug. The triple bioactivity high-resolution profiles were used to pinpoint bioactive compounds, and subsequent structure elucidation was performed with hyphenated......In this work, development of a new microplate-based high-resolution profiling assay using recombinant human aldose reductase is presented. Used together with high-resolution radical scavenging and high-resolution α-glucosidase assays, it provided the first report of a triple aldose reductase...

  11. The role of visual acuity and segmentation cues in compound word identification

    Directory of Open Access Journals (Sweden)

    Jukka eHyönä

    2012-06-01

    Full Text Available Studies are reviewed that demonstrate how the foveal area of the eye constrains how compound words are identified during reading. When compound words are short, their letters can be identified during a single fixation, leading to the whole-word route dominating word recognition from early on. Hence, visually marking morpheme boundaries by hyphens slows down processing by encouraging morphological decomposition when holistic processing is a feasible option. In contrast, the decomposition route dominates the early stages of identifying long compound words. Thus, visual marking of morpheme boundaries facilitates processing of long compound words, unless the initial fixation made on the word lands very close to the morpheme boundary. The reviewed pattern of results is explained by the visual acuity principle (Bertram & Hyönä, 2003 and the dual-route framework of morphological processing.

  12. Validated HPLC-RI method for the determination of lactulose and its process related impurities in syrup

    Directory of Open Access Journals (Sweden)

    Nelofar A

    2010-01-01

    Full Text Available A simple, swift with good sensitivity and reproducibility, HPLC-RI method has been developed for the quantification of lactulose and related compounds (fructose, galactose, epilactose and lactose in oral suspension formulation. The analysis was carried out by using mobile phase (water and acetonitrile 75:25 at the flow rate of 1.0 ml/min. on isocratic HPLC-RI system. After manipulating mobile phase composition and mobile phase flow rate a good separation of five components was achieved within 15 minutes of run time. This study is beneficial to determine the active ingredient as well as related compounds simultaneously, without using buffer in mobile phase which causes bad resolution and has limitation to analyze on other hyphenated techniques such as LC-MS.

  13. Structural elucidation of biologically active neomycin N-octyl derivatives in a regioisomeric mixture by means of liquid chromatography/ion trap time-of-flight mass spectrometry.

    Science.gov (United States)

    Giera, Martin; de Vlieger, Jon S B; Lingeman, Henk; Irth, Hubertus; Niessen, Wilfried M A

    2010-05-30

    Structural elucidation of six regioisomers of mono-N-octyl derivatized neomycin is achieved using MS(n) (up to n = 4) on an ion trap time-of-flight (IT-TOF) instrument equipped with electrospray ionization. The mixture of six derivatized neomycin analogues was generated by reductive amination in a shotgun synthetic approach. In parallel to the liquid chromatography/mass spectrometry (LC/MS) detection, the antibacterial activity of the neomycin regioisomers was tested by post-column addition of buffer and bacterial inocula, subsequent microfractionation of the resulting mixture, incubation, and finally a chemiluminescence-based bioactivity measurement based on the production of bacterial ATP. The MS-based high-resolution screening approach described can be applied in medicinal chemistry to help in designing and producing new antibiotic substances, which is particularly challenging due to the high functionality of most antibiotic substances, therefore requiring advanced (hyphenated) separation and detection techniques for compound mixtures.

  14. Mental illness in the nursing workplace: a collective autoethnography.

    Science.gov (United States)

    Kidd, Jacquie Dianne; Finlayson, Mary P

    2010-01-01

    Many nurses are burned out, exhausted and have a high intent to leave their jobs. These factors, when experienced over a period of time, are consistent with the development of mental illness. This study takes a collective autoethnographical approach to mental illness in the nursing workplace by focusing on the stories of nurses who have experienced mental illness in clinical practice. It highlights three ways in which nursing and mental illness are connected; the nurse who is vulnerable to mental illness prior to entering the profession, the nurse who develops mental illness that is independent of her work but is nevertheless impacted by it, and the nurse who develops mental illness as a result of her work and/or role. This paper explores the hyphenated lives and bullying these nurses experience, and recommends strategies that the profession, employing organisations, and individuals can adopt to reduce nurses' progression from stress to distress and mental illness.

  15. Apolar Compounds in Seaweeds from Fernando de Noronha Archipelago (Northeastern Coast of Brazil)

    Science.gov (United States)

    Ferreira, Leandro De Santis; Turatti, Izabel Cristina Casanova; Lopes, Norberto Peporine; Guaratini, Thais; Colepicolo, Pio; Oliveira Filho, Eurico Cabral; Garla, Ricardo Clapis

    2012-01-01

    Hyphenated techniques of gas chromatography coupled to mass spectrometer were used to determine fatty acids in eleven species of seaweeds from Fernando de Noronha archipelago. The main compounds detected in all studied species were the alcohol phytol and the fatty acids 14 : 0; 15 : 0; 16 : 0; 18 : 0; 18 : 1 n9; 18 : 2 Δ9,12; 20 : 4; 20 : 5. These fatty acids are commonly found in seaweeds present in warm regions. Thus, we found no specificity in the presence of a particular set of fatty acids and the studied species indicating that they are not useful as taxonomic indicators. However, they could be used in a comparative study with algae found in polluted area because many of the studied seaweeds are widespread and Fernando de Noronha has low human influence. PMID:22272200

  16. LC-MS metabolomics from study design to data-analysis – using a versatile pathogen as a test case

    Directory of Open Access Journals (Sweden)

    Maya Berg

    2013-01-01

    Full Text Available Thanks to significant improvements in LC-MS technology, metabolomics is increasingly used as a tool to discriminate the responses of organisms to various stimuli or drugs. In this minireview we discuss all aspects of the LC-MS metabolomics pipeline, using a complex and versatile model organism, Leishmania donovani, as an illustrative example. The benefits of a hyphenated mass spectrometry platform and a detailed overview of the entire experimental pipeline from sampling, sample storage and sample list set-up to LC-MS measurements and the generation of meaningful results with state-of-the-art data-analysis software will be thoroughly discussed. Finally, we also highlight important pitfalls in the processing of LC-MS data and comment on the benefits of implementing metabolomics in a systems biology approach.

  17. Recent trends in analytical methods and separation techniques for drugs of abuse in hair.

    Science.gov (United States)

    Baciu, T; Borrull, F; Aguilar, C; Calull, M

    2015-01-26

    Hair analysis of drugs of abuse has been a subject of growing interest from a clinical, social and forensic perspective for years because of the broad time detection window after intake in comparison to urine and blood analysis. Over the last few years, hair analysis has gained increasing attention and recognition for the retrospective investigation of drug abuse in a wide variety of contexts, shown by the large number of applications developed. This review aims to provide an overview of the state of the art and the latest trends used in the literature from 2005 to the present in the analysis of drugs of abuse in hair, with a special focus on separation analytical techniques and their hyphenation with mass spectrometry detection. The most recently introduced sample preparation techniques are also addressed in this paper. The main strengths and weaknesses of all of these approaches are critically discussed by means of relevant applications. PMID:25542354

  18. Synchrotron radiation for direct analysis of metalloproteins on electrophoresis gels.

    Science.gov (United States)

    Ortega, Richard

    2009-03-01

    Metalloproteomics requires analytical techniques able to assess and quantify the inorganic species in metalloproteins. The most widely used methods are hyphenated techniques, based on the coupling of a high resolution chromatographic method with a high sensitivity method for metal analysis in solution. An alternative approach is the use of methods for solid sample analysis, combining metalloprotein separation by gel electrophoresis and direct analysis of the gels. Direct methods are based on beam analysis, such as lasers, ion beams or synchrotron radiation beams. The aim of this review article is to present the main features of synchrotron radiation based methods and their applications for metalloprotein analysis directly on electrophoresis gels. Synchrotron radiation X-ray fluorescence has been successfully employed for sensitive metal identification, and X-ray absorption spectroscopy for metal local structure speciation in proteins. Synchrotron based methods will be compared to ion beam and mass spectrometry for direct analysis of metalloproteins in electrophoresis gels.

  19. Compound coverage enhancement of electrospray ionization mass spectrometry through the addition of a homemade needle.

    Science.gov (United States)

    Xiao, Shun; Qian, Shuai; Wang, Yi; Zhang, Yufeng; Cheng, Yiyu

    2013-03-21

    The response of many previously low-detectable or undetectable compounds in electrospray ionization mass spectrometry (ESI-MS) has been enhanced by the addition of a simple, homemade needle into the traditional ESI interface. The needle located between the ESI emitter and the ion sweep cone (inlet of the detector) would ionize those neutral gaseous compounds, formed during electrospray, by a corona discharge process. The mobile phases, ESI parameters and positions of the needle were investigated and optimized. Several groups of compounds and herbal extracts were tested using the homemade set-up. Both the results of the flow injection and the hyphenated MS analyses showed significant enhancement effects of our homemade needle. The advantages of the proposed method include low cost, simplicity and practicality. PMID:23364279

  20. Development of a micro flow-through cell for high field NMR spectroscopy.

    Energy Technology Data Exchange (ETDEWEB)

    Alam, Todd Michael; McIntyre, Sarah K.

    2011-05-01

    A highly transportable micro flow-through detection cell for nuclear magnetic resonance (NMR) spectroscopy has been designed, fabricated and tested. This flow-through cell allows for the direct coupling between liquid chromatography (LC) and gel permeation chromatography (GPC) resulting in the possibility of hyphenated LC-NMR and GPC-NMR. The advantage of the present flow cell design is that it is independent and unconnected to the detection probe electronics, is compatible with existing commercial high resolution NMR probes, and as such can be easily implemented at any NMR facility. Two different volumes were fabricated corresponding to between {approx}3.8 and 10 {micro}L detection volume. Examples of the performance of the cell on different NMR instruments, and using different NMR detection probes were demonstrated.

  1. Metallomics: the concept and methodology.

    Science.gov (United States)

    Mounicou, Sandra; Szpunar, Joanna; Lobinski, Ryszard

    2009-04-01

    The emerging field of metallomics refers to the entirety of research activities aimed at the understanding of the molecular mechanisms of metal-dependent life processes. This critical review discusses the concept of metallomics with a focus on analytical techniques and methods for the probing of interactions between metal ions and the organism's genome and the derived -omes: proteome and metabolome. Particular attention is paid to the in vivo screening for the native metal-protein and metal-metabolite complexes by hyphenated techniques that combine a high-resolution separation technique (gel electrophoresis, chromatography or capillary electrophoresis) with sensitive elemental (inductively coupled plasma, ICP) or molecular (electrospray or MALDI) mass spectrometric detection. The contribution of bioinformatics to the prediction of metal-binding sequences in proteins and the role of molecular biology approaches for the detection of metal-dependent genes, proteins and metabolites are highlighted (115 references).

  2. [Development of metallomics research on environmental toxicology].

    Science.gov (United States)

    Ogra, Yasumitsu

    2015-01-01

    Metallomics is newly coined terms and defined as a comprehensive analysis of the entirety of metal and metalloid species within a cell or tissue type. Then, metallome is defined as the entire category of metalloproteins and any other metal-containing biomolecules. Metallomics and research on metallome require analytical techniques that can provide information on the identification and quantification of metal/metalloid-containing biomolecules. This concept has been called speciation, and the acquisition of data according to the concept is performed using hyphenated techniques involving both separation and detection methods. In this review, the author intends to present several applications of complementary use of HPLC-inductively coupled plasma mass spectrometry (ICP-MS) and HPLC-electrospray ionization tandem mass spectrometry for identification of unknown selenium-containing metabolites, and also to present a newly developed technique, capillary LC-ICP-MS to be used for the analysis of metal-binding proteins.

  3. Automotive Painting Technology A Monozukuri-Hitozukuri Perspective

    CERN Document Server

    Salazar, Abraham; Saito, Kozo

    2013-01-01

    This book offers unique and valuable contributions to the field. It offers breadth and inclusiveness. Most existing works on automotive painting cover only a single aspect of this complex topic, such as the chemistry of paint or paint booth technology. Monozukuri and Hitozukuri are Japanese terms that can be translated as “making things” and “developing people” but their implications in Japanese are richer and more complex than this minimal translation would indicate. The Monozukuri-Hitozukuri perspective is drawn from essential principles on which the Toyota approach to problem-solving and continuous improvement is based. From this perspective, neither painting technology R&D nor painting technology use in manufacturing can be done successfully without integrating technological and human concerns involved with making and learning in the broadest sense, as the hyphen is meant to indicate. The editors provide case studies and examples -- drawn from Mr. Toda’s 33 years of experience with automotiv...

  4. International congress on analytical science for advanced material processing and environmental impact assessment

    International Nuclear Information System (INIS)

    The topics covered in the proceedings of the International Congress on Analytical Science 2010 include sampling and sample treatment pre-concentration (including solid phase extraction) organic analytical reagents, chemometrics, quality assurance/quality control, chromatography (GC, HPLC, IC, TLC etc.) and related techniques, hyphenated methods atomic spectroscopy (absorption, emission, fluorescence, XRF, XRD, lasers), molecular spectroscopy (IR, Raman), separation methods in analytical chemistry, sensors. Mass spectrometry, nuclear analytical methods, electroanalytical methods, geoanalytical chemistry, thermal analysis, process analytical chemistry, molecular probes for analyte sensing and imaging, express test methods, surface analytical methods, analytical microscopy, bioanalytical chemistry, environmental analysis, characterization of nano materials, analysis of new materials (including high-purity materials), analysis of food and agricultural products, clinical/forensic analysis, online analysis/process analytical chemistry, novel analytical techniques, lab on chips, LIMS, trace metal analysis and speciation. Papers relevant to INIS are indexed separately

  5. Identifying the tobacco related free radicals by UPCC-QTOF-MS with radical trapping method in mainstream cigarette smoke.

    Science.gov (United States)

    Wang, Ying; Liu, Misha; Zhu, Yingjing; Cheng, Kuan; Da Wu; Liu, Baizhan; Li, Fengting

    2016-11-01

    Tobacco related free radicals (TFRs) in the cigarette smoke are specific classes of hazardous compounds that merit concern. In this study, we developed a hybrid method to identify TFRs directly based on ultra-performance convergence chromatography with a quadrupole time-of-flight mass spectrometry (UPCC-QTOF MS) combined spin trapping technique. The short-lived TFRs were stabilized successfully in situ through spin trapping procedure and UPCC was applied to facilitate efficient separation of complex derivative products. Coupling of orthogonal partial least squares discriminant analysis (OPLS-DA), UPCC-QTOF MS system enabled us to identify specific potential TFRs with exact chemical formula. Moreover, computational stimulations have been carried out to evaluate the optimized stability of TFRs. This work is a successful demonstration for the application of an advanced hyphenated technique for separation of TFRs with short detection time (less than 7min) and high throughput.

  6. Capillary electrophoretic methods in the development of metal-based therapeutics and diagnostics: new methodology and applications.

    Science.gov (United States)

    Bytzek, Anna K; Hartinger, Christian G

    2012-02-01

    In recent years, capillary electrophoresis (CE) has matured to a standard method in medicinal inorganic chemistry. More and more steps of the drug discovery process are followed by CE. However, not only the number of applications has steadily increased but also the variety of used methodology has significantly broadened and, as compared to a few years ago, a wider scope of separation modes and hyphenated systems has been used. Herein, a summary of the newly utilized CE methods and their applications in metallodrug research in the timeframe 2006-2011 is presented, following related reviews from 2003 and 2007 (Electrophoresis, 2003, 24, 2023-2037; Electrophoresis 2007, 28, 3436-3446). Areas covered include impurity profiling, quality control of pharmaceutical formulations, lipophilicity estimation, interactions between metallodrugs and proteins or nucleotides, and characterization and also quantification of metabolites in biological matrices and real-world samples.

  7. A Review on Inductively Coupled Plasma Mass Spectroscopy

    Directory of Open Access Journals (Sweden)

    Ramyalakshmi G

    2012-12-01

    Full Text Available Inductively coupled plasma mass spectroscopy is routinely used in many diverse research fields such as earth, environmental, life and forensic sciences and in food, material, chemical, semiconductor and nuclear industries. The high ion density and the high temperature in a plasma provide an ideal atomizer and element ionizer for all types of samples and materials introduced by a specialised devices .outstanding properties such as high sensitivity, relative salt tolerance, compound-independent element response and highest quantitation accuracy lead to the unchallenged performance of ICPMS in efficiently detecting, identifying and reliably quantifying trace element. The increasing availability of relevant reference compounds and high separation selectively extend the molecular identification capability of ICPMS hyphenated to species – specific separation techniques

  8. Analytical developments in ICP-MS for arsenic and selenium speciation. Application to granitic waters

    International Nuclear Information System (INIS)

    Nuclear waste storage in geological areas needs the understanding of the physico-chemistry of groundwaters interactions with surrounding rocks. Redox potential measurements and speciation, calculated from geochemical modelling are not significant for the determination of water reactivity. We have thus chosen to carry out experimental speciation by developing sensitive analytical tools with respect of specie chemical identity. We have studied two redox indicators from reference sites (thermal waters from Pyrenees, France): arsenic and selenium. At first, we have determined the concentrations in major ions (sulphide, sulphate, chloride, fluoride, carbonate, Na, K, Ca). Speciation was conducted by HPLC hyphenated to quadrupole ICP-MS and high resolution ICP-MS. These analyses have shown the presence of two new arsenic species in solution, in addition of a great reactivity of these waters during stability studies. A sampling, storage and analysis method is described. (author)

  9. Gas chromatography-mass spectrometry metabolomics of goat milk with different polymorphism at the αS1-casein genotype locus.

    Science.gov (United States)

    Caboni, Pierluigi; Murgia, Antonio; Porcu, Alessandra; Demuru, Martina; Pulina, Giuseppe; Nudda, Anna

    2016-08-01

    Hyphenated gas chromatography-mass spectrometry (GC-MS) and multivariate data analysis techniques were used to uncover milk metabolite differences in different αS1-casein genotypes of goats. By a discriminant GC-MS metabolomics approach, we characterized milk polar metabolites of 28 goats. Animals were selected on the basis of their genotypes as 7 goats classified heterozygous for weak or null alleles, 5 for the genotype EE, 9 for the genotypes AE and BE, and finally 7 for the strong genotype AA. Low molecular weight polar metabolite profile was tightly related to the different goat genotypes, milk production, and protein levels. Results of multivariate statistical analysis of GC-MS data demonstrate that different heterozygous and homozygous genotypes expressed different metabolites such as citric and aconitic acid for the strong allele class with different sugars and polyols for the weak class. PMID:27289154

  10. Qualitative and quantitative analysis of branches in dextran using high-performance anion exchange chromatography coupled to quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Yi, Lin; Ouyang, Yilan; Sun, Xue; Xu, Naiyu; Linhardt, Robert J; Zhang, Zhenqing

    2015-12-01

    Dextran, a family of natural polysaccharides, consists of an α (1→6) linked-glucose main (backbone) chain having a number of branches. The determination of the types and the quantities of branches in dextran is important in understanding its various biological roles. In this study, a hyphenated method using high-performance anion exchange chromatography (HPAEC) in parallel with pulsed amperometric detection (PAD) and mass spectrometry (MS) was applied to qualitative and quantitative analysis of dextran branches. A rotary cation-exchange cartridge array desalter was used for removal of salt from the HPAEC eluent making it MS compatible. MS and MS/MS were used to provide structural information on the enzymatically prepared dextran oligosaccharides. PAD provides quantitative data on the ratio of enzyme-resistant, branched dextran oligosaccharides. Both the types and degree of branching found in a variety of dextrans could be simultaneously determined online using this method.

  11. Developments and trends in inductively coupled plasma mass spectrometry and its influence on the recent advances in trace element analysis

    International Nuclear Information System (INIS)

    A brief introduction to the various instrumental methods such as atomic absorption spectrometry, x-ray fluorescence spectrometry, neutron activation analysis, inductively coupled plasma atomic emission spectrometry, thermal ionization mass spectrometry, etc. are presented highlighting their relative merits and demerits. The history and developments of inductively coupled plasma mass spectrometry (ICP-MS) and its advantages and limitations over other multi-element instrumental techniques are reviewed. Extended capabilities by hyphenating ICP-MS to various other well-known sample introduction techniques such as flow-injection, electrothermal vaporization, chromatographic methods and laser ablation are discussed in brief. The recent development of high resolution multi-collector double-focusing magnetic mass spectrometer with inductively coupled plasma at atmospheric pressure as source is also discussed. Some of the areas where more developments can be expected in future are suggested. (author). 77 refs., 4 tabs., 3 figs

  12. Novel applications of high performance ion chromatography-inductively coupled plasma mass spectrometry (HPIC-ICP-MS)

    International Nuclear Information System (INIS)

    This work demonstrates the development of highly sensitive and selective analytical methods, which make use of the hyphenation of high performance ion chromatography (HPIC) to inductively coupled plasma sector field mass spectrometry (ICP-SFMS). On-line coupling a chromatographic separation method with an elemental detection method provides two advantages: (1) the components of a possibly interfering matrix can be separated allowing accurate and precise ultra trace analysis of the element of interest and (2) elemental species of an element can be separated and quantified. In this work, matrix separation methods for interference free determination of 232Th, 234U, 235U and 238U in geological matrices were developed and employed. Furthermore HPIC-ICP-SFMS was applied for ultra trace analysis of Pd in environmental and geological matrices. The usefulness of HPIC-ICP-SFMS for speciation studies was demonstrated by investigating the interaction of an anti-cancer drug (cisplatin) with guanosine monophosphates. (author)

  13. Novel applications of high performance ion chromatography - inductively coupled plasma mass spectrometry (HPIC-ICP-MS)

    International Nuclear Information System (INIS)

    This work demonstrates the development of highly sensitive and selective analytical methods, which make use of the hyphenation of high performance ion chromatography (HPIC) to inductively coupled plasma sector field mass spectrometry (ICP-SFMS). On-line coupling a chromatographic separation method with an elemental detection method provides two advantages: (1) The components of a possibly interfering matrix can be separated allowing accurate and precise ultra trace analysis of the element of interest and (2) elemental species of an element can be separated and quantified. In this work, matrix separation methods for interference free determination of 232Th, 234U, 235U and 238U in geological matrices were developed and employed. Furthermore HPIC-ICP-SFMS was applied for ultra trace analysis of Pd in environmental and geological matrices. The usefulness of HPIC-ICP-SFMS for speciation studies was demonstrated by investigating the interaction of an anti-cancer drug (cisplatin) with guanosine monophosphates. (author)

  14. Chlorococcalean microalgae Ankistrodesmus convolutes biodiesel characterization with Fourier transform-infrared spectroscopy and gas chromatography mass spectroscopy techniques

    Directory of Open Access Journals (Sweden)

    Swati SONAWANE

    2015-12-01

    Full Text Available The Chlorococcalean microalgae Ankistrodesmus convolutes was found in fresh water Godawari reservoir, Ahmednagar district of Maharashtra State, India. Microalgae are modern biomass for the production of liquid biofuel due to its high solar cultivation efficiency. The collection, harvesting and drying processes were play vital role in converting algal biomass into energy liquid fuel. The oil extraction was the important step for the biodiesel synthesis. The fatty acid methyl ester (FAME synthesis was carried through base catalyzed transesterification method. The product was analyzed by using the hyphened techniques like Fourier Transform-Infrared spectroscopy (FT-IR and Gas Chromatography Mass Spectroscopy (GCMS. FT-IR Spectroscopy was results the ester as functional group of obtained product while the Gas Chromatography Mass Spectroscopy was results the six type of fatty acid methyl ester with different concentration. Ankistrodesmus convolutes biodiesel consist of 46.5% saturated and 49.14% unsaturated FAME.

  15. Chromium interactions in plants: current status and future strategies.

    Science.gov (United States)

    Shanker, Arun Kumar; Djanaguiraman, Maduraimuthu; Venkateswarlu, Bandi

    2009-09-01

    Chromium has received relatively little attention from plant scientists compared to other heavy metals in recent times in spite of it being a very a hazardous environmental pollutant. One of the reasons for this is the complexity of the metal's interactions with biological systems and the difficulty in studying them. Although the possible mode of entry into the plants, resultant toxicity mechanisms and tolerance potential has been worked out in plants there is still a need to get a complete picture of the Cr-plant interactome. With the advent of hyphenated technologies and global gene/protein and metabolite expression/quantification techniques, studies to elucidate the complete metallome are possible albeit resource intensive. This minireview focuses on the recent developments in the field of Cr-plant interactions and proposes a model using a systems biology and integrated -omics approach to decipher the intricacies of Cr-plant interaction. PMID:21305140

  16. Development and Applications of Liquid Sample Desorption Electrospray Ionization Mass Spectrometry

    Science.gov (United States)

    Zheng, Qiuling; Chen, Hao

    2016-06-01

    Desorption electrospray ionization mass spectrometry (DESI-MS) is a recent advance in the field of analytical chemistry. This review surveys the development of liquid sample DESI-MS (LS-DESI-MS), a variant form of DESI-MS that focuses on fast analysis of liquid samples, and its novel analy-tical applications in bioanalysis, proteomics, and reaction kinetics. Due to the capability of directly ionizing liquid samples, liquid sample DESI (LS-DESI) has been successfully used to couple MS with various analytical techniques, such as microfluidics, microextraction, electrochemistry, and chromatography. This review also covers these hyphenated techniques. In addition, several closely related ionization methods, including transmission mode DESI, thermally assisted DESI, and continuous flow–extractive DESI, are briefly discussed. The capabilities of LS-DESI extend and/or complement the utilities of traditional DESI and electrospray ionization and will find extensive and valuable analytical application in the future.

  17. Notas sobre a liberdade e a tirania da maioria em Stuart Mill

    Directory of Open Access Journals (Sweden)

    Antonio Ozaí da Silva

    2009-10-01

    Full Text Available O liberalismo é uma doutrina política que, em suas origens, tem como alicerce vários autores clássicos do pensamento político: Locke, Montesquieu, Kant, Adam Smith, Humboldt, Benjamin Constant, Alexis de Tocqueville, Stuart Mil e outros. Portanto, a exemplo do socialismo, cabe perfeitamente a pergunta: Qual liberalismo? Como o(s marxismo(s, o pensamento liberal não é homogêneo. Da mesma forma, o conceito de liberdade no pensamento liberal tem mais de uma conotação, como também a sua crítica. Estes apontamentos se limitam a expor o pensamento político de John Stuart Mill, mais precisamente sobre a sua argumentação em defesa da liberdade individual e a crítica à tirania da maioria no ensaio “Sobre a Liberdade” (MILL, 1991.

  18. Um gramsciano a serviço da união dos povos

    Directory of Open Access Journals (Sweden)

    Marco Aurélio Nogueira

    2010-02-01

    Full Text Available Quarta-feira, 20 de janeiro, soube da morte de Giorgio Baratta. Poucos brasileiros sabem quem foi ele. Era conhecido e admirado por marxistas gramscianos, com quem mantinha relações estreitas, aqui no Brasil e em diversas partes do mundo. A todos encantava com sua ironia fina, seu conhecimento enciclopédico, sua admiração incondicional por Gramsci – uma admiração que não o cegava nem o fechava em tolos dogmatismos.

  19. As bregafestas de fim de ano (apenas uma reflexão pessoal

    Directory of Open Access Journals (Sweden)

    Raymundo de Lima

    2010-01-01

    Full Text Available Peço perdão aos festeiros de fim de ano, pela minha irritação com o mesmismo dessa época. Acho horrorosas as musiquinhas com arpa, os anúncios televisivos, os enfeites bregaluminosos nas árvores urbanas, as filas, a obrigação de desejar feliz Natal e Próspero Ano Novo, receber-enviar mensagens etc. Na verdade, me irrito com o consumismo e a profanação do significado do nascimento de Jesus. Incomodo-me especialmente com as mulheres que entram em frenesi com as compras de roupas pra si, para parentes e crianças exigentes com presentes de griffes, a ansiedade dos preparativos para a ceia de Natal, seleção dos convidados. Por que ceia? Por que “tem que ter” peru? No Rio “tem que ter” rabanada gordurosa?

  20. O desafio social do saber universitário

    Directory of Open Access Journals (Sweden)

    Moisés dos Santos Viana

    2009-08-01

    Full Text Available O artigo é uma reflexão sobre o saber universitário e o desafio social de gerar conhecimento técnico-científico. Desse modo, há muitas implicações e divergências em meio ao conhecimento e seu aspecto emancipador. Uma crítica ao utilitarismo universitário, mercadológico, que se manifesta como práxis conservadora do status quo. Assim, propõem-se um novo modo de refletir, sentir, dialogar, agir para provocar, alterar e superar o desafio social do saber universitário.    

  1. Articles with short titles describing the results are cited more often

    Directory of Open Access Journals (Sweden)

    Carlos Eduardo Paiva

    2012-01-01

    Full Text Available OBJECTIVE: The aim of this study was to evaluate some features of article titles from open access journals and to assess the possible impact of these titles on predicting the number of article views and citations. METHODS: Research articles (n = 423, published in October 2008 from all Public Library of Science (PLoS journals and from 12 Biomed Central (BMC journals were evaluated. Publication metrics (views and citations were analyzed in December 2011. The titles were classified according to their contents, namely methods-describing titles and results-describing titles. The number of title characters, title typology, the use of a question mark, reference to a specific geographical region, and the use of a colon or a hyphen separating different ideas within a sentence were analyzed to identify predictors of views and citations. A logistic regression model was used to identify independent title characteristics that could predict citation rates. RESULTS: Short-titled articles had higher viewing and citation rates than those with longer titles. Titles containing a question mark, containing a reference to a specific geographical region, and that used a colon or a hyphen were associated with a lower number of citations. Articles with results-describing titles were cited more often than those with methods-describing titles. After multivariate analysis, only a low number of characters and title typology remained as predictors of the number of citations. CONCLUSIONS: Some features of article titles can help predict the number of article views and citation counts. Short titles presenting results or conclusions were independently associated with higher citation counts. The findings presented here could be used by authors, reviewers, and editors to maximize the impact of articles in the scientific community.

  2. Recent advances and trends in the liquid-chromatography-mass spectrometry analysis of flavonoids.

    Science.gov (United States)

    de Villiers, André; Venter, Pieter; Pasch, Harald

    2016-01-22

    Flavonoids have elicited significant attention as a result of their importance in plants, their influence on the properties of natural-product derived commodities and especially as a consequence of their purported health benefits. Research in all of these fields relies heavily on accurate analytical data, and in this LC-MS has come to play an influential role by allowing relatively fast tentative identification and accurate quantification of low levels of flavonoids in a variety of matrices. The field has undergone rapid expansion in the last decade due to important developments in both HPLC and MS instrumentation, which nowadays allow much faster and more accurate analysis of flavonoids. This contribution aims to provide an overview of these developments and their application in flavonoid analysis since 2009. The discussion is focussed first on methodologies which provide improved LC separation of flavonoids in terms of speed and/or resolution, including ultra high pressure LC (UHPLC), monolithic and superficially porous phases, high temperature LC (HTLC) and comprehensive two-dimensional LC (LC×LC). The fundamental background relevant to each of these will be briefly outlined, as well as the implications and promise of their hyphenation to MS. Secondly, the possibilities and limitations of a range of the latest MS instruments available in combination with advanced LC analysis will be discussed, including ion trap, triple quadrupole, time-of-flight, Orbitrap, ion mobility and various hybrid instruments. Examples from the latest literature will be used to illustrate the performance gains achievable in flavonoid analysis by the hyphenation of advanced LC separation and high-end MS instrumentation.

  3. Steam Methane Reforming System for Hydrogen Production: Advanced Exergetic Analysis

    Directory of Open Access Journals (Sweden)

    Tatiana Morosuk

    2012-02-01

    Full Text Available Steam methane reforming (SMR is one of the most promising processes for the production of hydrogen. Therefore, the overall thermodynamic efficiency of this process is of particular importance. The thermodynamic inefficiencies in a thermal system are related to exergy destruction and exergy loss. However, a conventional exergetic analysis cannot evaluate the mutual interdependencies among the system components nor the real potential for improving the energy conversion system being considered. One of the tools under development for the improvement of energy conversion systems from the thermodynamic viewpoint is the advanced exergetic analysis. In this paper, the avoidable part of the exergy destruction is estimated and the interactions among components of the overall system are evaluated in terms of endogenous and exogenous exergy destruction. The assumptions required for these calculations are discussed in detail, especially for those components that are typically used in chemical processes. Results of this paper suggest options for increasing the thermodynamic efficiency of hydrogen production by steam-methane reforming.

  4. User Experience – Essencial para Usabilidade de Produtos

    Directory of Open Access Journals (Sweden)

    Antonio Mendes Silva Filho

    2011-07-01

    Full Text Available Usabilidade tem sido um dos fatores utilizados por empresas para conquistar novos usuários (consumidores. De acordo com a Norma 9241-11 da ISO (International Organization for Standardization, a usabilidade é definida como “The extent to which a product can be used by specified users to achieve specified goals with effectiveness, efficiency, and satisfaction in a specified context of use”. Esses objetivos compreendem a base do que é denominado “user experience”. Mas, o que é user experience? Trata-se da experiência do usuário quando interage com produtos ou serviços. Um produto pode ser qualquer coisa como, por exemplo, um notebook, um aparelho celular ou smartphone, um painel de automóvel ou software. Qualquer desses produtos ou até serviços (como oferecidos em web sites, têm a usabilidade como atributo determinante da qualidade perceptível aos usuários. Nesse sentido, o objetivo deste artigo é discutir e explorar experiência e percepção do usuário no uso e adoção de novas tecnologias. O artigo destaca como a Apple tem inovado em seus produtos provendo usabilidade levando em consideração a experiência do usuário.

  5. Ministério do Turismo e sua Festa de Babette

    Directory of Open Access Journals (Sweden)

    João dos Santos Filho

    2010-05-01

    Full Text Available Não sei por que! Mas quando estava pensando na Política Nacional de Turismo, visualizei um banquete, onde a prática gastronômica explicitava inexistir a plena felicidade sem o pecado, que pode ser o da gula em razão da comida e do dinheiro pela existência das emendas parlamentares. O Ministério do Turismo seria madame Babette em seu banquete articulado por um maquiamento marqueteiro, buscando contrapor a noção do pecado com a idéia da felicidade.

  6. Relevance of two-dimensional gas chromatography and high resolution olfactometry for the parallel determination of heat-induced toxicants and odorants in cooked food.

    Science.gov (United States)

    Giri, Anupam; Khummueng, Weeraya; Mercier, Frédéric; Kondjoyan, Nathalie; Tournayre, Pascal; Meurillon, Maïa; Ratel, Jérémy; Engel, Erwan

    2015-04-01

    The assessment of the dual impact of heating treatments on food safety and aroma is a major issue for the food sector. The aim of the present study was to demonstrate the relevance of multidimensional GC techniques, olfactometry and mass spectrometry for the parallel determination of process-induced toxicants and odorants in food starting with cooked meat as a food model. PAHs were analyzed by comprehensive two-dimensional gas chromatography-time-of-flight mass spectrometry after extraction by accelerated solvent extraction (ASE-GC × GC-TOF/MS). Odour-active compounds were determined by dynamic headspace-GC hyphenated with eight booth olfactometry and mass spectrometry (DH-GC-MS/8O) and DH-heart-cutting multidimensional GC hyphenated with olfactometry and mass spectrometry (DH-GC-GC-MS/O). For PAH determination, the GC × GC conditions consisted of a combination of a primary non-polar BPX-5 column and a secondary polar BPX-50 column, and a modulation period of 5s. In terms of linearity (R(2) ranging from 0.985 to 0.997), recovery rate (84-111%) and limit of detection (5-65 ng/kg of cooked meat), the ASE-GC × GC-TOF/MS method was found consistent with the multiresidue determination of 16 PAHs including benzo[a]pyrene in cooked meat. For aroma compounds, DH-GC-MS/8O and DH-GC-MS/O revealed 53 major meat odour-active compounds. A customized heart-cutting GC-GC-MS/O enabled the coeluting odour zones with high odour-activity to be resolved and revealed 15 additional odour-active compounds. Finally, these developments of multidimensional approaches were used to investigate the balance between 16 PAHs and 68 odour-active compounds generated with different cooking techniques. PMID:25728653

  7. Online coupling solid-phase ligand-fishing with high-performance liquid chromatography-diode array detector-tandem mass spectrometry for rapid screening and identification of xanthine oxidase inhibitors in natural products.

    Science.gov (United States)

    Peng, Mi-Jun; Shi, Shu-Yun; Chen, Lin; Zhang, Shui-Han; Cai, Ping; Chen, Xiao-Qing

    2016-09-01

    Screening and analysis of bioactive compounds from natural products is challenging work due to their complexity. This study presents the first report on hyphenation of solid-phase ligand-fishing using immobilized xanthine oxidase microcolumn (IXOM) and high-performance liquid chromatography-diode array detector-tandem mass spectrometry (HPLC-DAD-MS/MS) for screening and identification of XO inhibitors from complex mixtures. Solid-phase ligand-fishing system was hyphenated with the HPLC system via four-port switching valve and a six-port injection valve as an interface for transferring effluents from IXOM to HPLC, and collecting chromatograms from LFMC (ligand-fishing microextraction column) and C18 column in a run by only one DAD. Mixtures containing allopurinol (positive control) and tryptophane (negative control) were analyzed in order to verify the specificity and reproducibility of the approach. Subsequently, the newly developed system was applied to screening and identification of XO inhibitors from L. macranthoides and its human microsomal metabolites. Six prototype compounds (3-caffeoylquinic acid, 5-caffeoylquinic acid, 4-caffeoylquinic acid, 3,4-dicaffeoylquinic acid, 3,5-dicaffeoylquinic acid, 4,5-dicaffeoylquinic acid) and three metabolites (3-caffeoyl-epi-quinic acid, 5-caffeoyl-epi-quinic acid, 4-caffeoyl-epi-quinic acid) with XO binding affinities were identified. The XO inhibition activities of six prototype compounds were evaluated and confirmed using in vitro enzymatic assay. With the online system developed here, we present a feasible, selective, and effective strategy for rapid screening and identification of enzyme inhibitors from complex mixtures. PMID:27438719

  8. O Muro, dois Estados, dois Mundos

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    Luis Edmundo de Souza Moraes

    2009-11-01

    Full Text Available

    O  artigo trata do problema das fronteiras sociais e políticas na Berlim do pós-II Guerra Mundial relacionadas à divisão da cidade em zonas de ocupação e, posteriormente, à construção do Muro. Ele reflete sobre o fato de que o muro, que dividiu uma cidade de forma artificial, produziu divisões e diferenças concretas pela ação do tempo, criando descontinuidades onde haviam continuidades. O artigo ainda aponta para uma forma de pensar o encontro não planejado entre as duas partes da cidade naquilo que foi chamada de reunificação.

  9. Étude préliminaire sur les stucs trouvés dans le "Bâtiment à Péristyle" du quartier sud-ouest de Palmyre (PAL.M.A.I.S. - Fouilles 2008-2009 A preliminary study on the stuccos found in the "Peristyle Building" of Palmyra's south-west quarter (PAL.M.A.I.S. - Excavations 2008-2009

    Directory of Open Access Journals (Sweden)

    Lilia Palmieri

    2011-03-01

    Full Text Available

    The Italian-Syrian joint Mission of the Università degli Studi of Milan at Palmyra (Pal.M.A.I.S. = Palmira. Missione Archeologica Italo-Siriana is focus on the exploration of the south-west quarter of the ancient city. Since 2008 the stratigraphic excavation of the "Peristyle Building" has begun. Many fragments of stucco which are part of a frieze decorated by an Anthemion have been found in one room of the building - the room A -. These fragments belong to the decoration of a luxury complex which was damaged (or destroyed? before the 6th century AD, and they are very important elements in order to define the chronological horizon of the first phase of development of the area.

    Les travaux archéologiques de la Mission conjointe italienne-syrienne de l'Università degli Studi de Milan à Palmyre (Pal.M.A.I.S.= Palmira. Missione Archeologica Italo-Siriana sont dédiés à l’exploration du quartier sud-ouest de la ville antique. Depuis 2008 a été entreprise la fouille stratigraphique du "Bâtiment à Péristyle", et dans une

  10. A proposito di arredi. Prima e dopo la tenda di Tolomeo Filadelfo About furniture. Before and after Ptolomaeus Philadelphos' pavilion

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    Elena Calandra

    2010-07-01

    Full Text Available

    The furniture is of primary importance towards the canopies definition, more than the architectonic structure: they  contribute, in fact, in creating and organizing the spaces, so that there is almost no distinction between furniture and structure, as it is possible to observe in the ancient sources of different periods (Herodotus, Euripides, Julius Caesar, Plutarchus, Athenaeus: the pavilions of Xerxes at Plataia, of Ion at Delphi, of Alexander after the Issa battle and at Susa, of Pompey at Pharsalos, as well as the Ptolomaeus's canopy at Alexandria.

    At the same time, the furniture language is studied, signifying the power and the force of the sovereign through the luxurious materials and surprising the spectators.

         At the end, some hypotheses on the final destination of the furniture, after dismantling the Ptolomaeus' canopy, equiped for one year. 

    Soil biochemical attributes can be used as sensitive indicators of alterations promoted by the agricultural use, being a tool to guide tillage practices planning and evaluation to maintain soil sustainability. The objective of this study was to evaluate alterations in the soil organic carbon, biomass and microbial activity, urease and acid phosphatase activity, in two savannah soils, as affected by soil management systems. The study consisted of five soil management systems in a Typic Quartzipsamment, four in an Oxisol, and reference areas without alterations in the two soil types. The management systems changed the biochemical attributes of both soils. The Typic Quartzipsamment area under the soybean/Brachiaria decumbens sequence decreased the soil organic carbon and the microbial biomass carbon, and increased the respiration and qCO2, while the Oxisol, in all the areas, except for pasture, promoted reductions in the biochemical attributes. Among the management systems studied,  the pasture provided improvements in the evaluated attributes, in both soils.

    KEY-WORDS: Soil quality; microbial biomass; soil enzymatic activity.

    The article questions the usual views on migration, which characterize it merely as the provisional movement of foreign labor and obscure its fundamentally political meaning

  11. Exergoeconomic optimization of an Organic Rankine Cycle for low-temperature geothermal heat sources

    Directory of Open Access Journals (Sweden)

    Dieter Brüggemann

    2012-05-01

    Full Text Available

    An exergoeconomic analysis of a geothermal power generation for a low-temperature resource is performed. An Organic Rankine Cycle (ORC with isobutane and isopentane as working fluids is considered as binary power plant. A systematic parameter variation is done for the minimum temperature difference in the evaporator and condenser. The most suitable design parameters are evaluated under exergetic, economic and exergoeconomic criteria. The specific costs of electricity generation are minimal for the use of isobutane as working fluid and minimal temperature difference of 3 K at evaporation and 7 K at condensation. The most suitable concept for isopentane leads to only 0.4

  12. Afinidades eletivas: EZLN e MST na contramão da história do progresso dos vencedores

    Directory of Open Access Journals (Sweden)

    Fabio Querido

    2011-04-01

    Full Text Available

    Inspirando-se em algumas reflexões de Walter Benjamin e, em menor medida, de José Carlos Mariátegui, o objetivo deste pequeno artigo é esboçar algumas afinidades eletivas entre o Exército Zapatista de Libertação Nacional e o Movimento dos Trabalhadores Sem Terra, particularmente no que se refere à importância que eles conferem ao resgate e rememoração das lutas sociais do passado – transformadas em fonte de inspiração das lutas do presente.

  13. Separation of pigment formulations by high-performance thin-layer chromatography with automated multiple development.

    Science.gov (United States)

    Stiefel, Constanze; Dietzel, Sylvia; Endress, Marc; Morlock, Gertrud E

    2016-09-01

    Food packaging is designed to provide sufficient protection for the respective filling, legally binding information for the consumers like nutritional facts or filling information, and an attractive appearance to promote the sale. For quality and safety of the package, a regular quality control of the used printing materials is necessary to get consistently good print results, to avoid migration of undesired ink components into the food and to identify potentially faulty ink batches. Analytical approaches, however, have hardly been considered for quality assurance so far due to the lack of robust, suitable methods for the analysis of rarely soluble pigment formulations. Thus, a simple and generic high-performance thin-layer chromatography (HPTLC) method for the separation of different colored pigment formulations was developed on HPTLC plates silica gel 60 by automated multiple development. The gradient system provided a sharp resolution for differently soluble pigment constituents like additives and coating materials. The results of multi-detection allowed a first assignment of the differently detectable bands to particular chemical substance classes (e.g., lipophilic components), enabled the comparison of different commercially available pigment batches and revealed substantial variations in the composition of the batches. Hyphenation of HPTLC with high resolution mass spectrometry and infrared spectroscopy allowed the characterization of single unknown pigment constituents, which may partly be responsible for known quality problems during printing. The newly developed, precise and selective HPTLC method can be used as part of routine quality control for both, incoming pigment batches and monitoring of internal pigment production processes, to secure a consistent pigment composition resulting in consistent ink quality, a faultless print image and safe products. Hyphenation of HPTLC with the A. fischeri bioassay gave first information on the bioactivity or rather

  14. Conventional Exergetic and Exergoeconomic Analyses of a Power Plant with Chemical Looping Combustion for CO2 Capture

    Directory of Open Access Journals (Sweden)

    Tatiana Morosuk

    2010-09-01

    Full Text Available

    Exergy-based methods can be used as a tool for examining, comparing and assessing thermodynamic systems. In this paper, an exergoeconomic analysis is used to evaluate a power plant with chemical looping combustion (CLC for CO2 capture. This oxy-fuel plant is compared, from an exergetic and an economic perspective, to a conventional, reference power plant without CO2 capture. The exergetic analysis shows decreased exergy destruction in the CLC reactors, compared to the exergy destruction in the conventional combustion chamber of the reference case; thus, the irreversibilities caused by combustion in the CLC are reduced. However, due to the addition of the CO2 compression unit, the overall exergetic efficiency of the plant with CLC is lower than that of the reference plant by approximately 5 percentage points. The economic analysis confirms a significant increase in the investment cost of the CO2 capture plant, due to the addition of the units for CO2 compression and CLC. Thus, the cost of electricity is 24% higher for this plant in comparison to that of the reference case. Nevertheless, when compared to the reference plant with CO2 capture with monoethanolamine, the plant with CLC was found to be a more economical option. Since CO2 abatement must be realized in the future, given expected environmental or tax measures, CLC provides relatively low cost carbon dioxide capture and it, therefore, appears to be a promising option for

  15. NatureDNS:一种自然语言式域名寻址系统%NATUREDNS: AN ADDRESSING SYSTEM FOR DOMAIN NAMES USING NATURAL LANGUAGES

    Institute of Scientific and Technical Information of China (English)

    刘振兴

    2013-01-01

    探讨一种使用自然语言进行域名注册登记、解析和寻址的方法.现行的域名系统DNS(Domain Name System)采用层级式的命名空间,点分多段表达式,域名与IP的对应关系维护在一个分布式的数据库系统中.随着网络发展这种体系面临:(1)越来越多的人们被迫接受一种点分字符串作为访问对象的标记;(2)随着新顶级域名的增多和国际化域名的启用,点分字符串的域名变得进一步复杂多变.在深入分析这一体系及其他相关改进型探索的基础上,提出一种以“-”(hyphen)为起始和分级标记使用自然语言式字符串进行网络寻址的新方法(“-XXXX”),取名为NatureDNS,即“自然语言式DNS系统”.%We propose an approach for registration, resolution and addressing of the domain names using natural languages. Current DNS is a hierarchical namespace where the dotted multi-segment expression, the correlated relationship of domain name and its IP addresses are maintained in a distributed database system. With the development of the networks, such system is encountering: 1) more and more people are compelled to accept the dotted strings as the tags for the accessing objects; 2) along with the increasing of new gTLD and the enabling of the IDN, the domain names with dotted strings become more complicated and changeable than ever. Based on a thorough investigation on this system and other related improvement exploration, we present in the article a new method ( "-xxxx" ) , which uses "-" ( hyphen) as the tags of starting and hierarchical separation, and uses natural languages string for networks addressing, and give its name as "NatureDNS" , i. e. , "to express the domain names in natural languages".

  16. O Ensino do Sistema de Escrita Alfabética: PCN de Língua Portuguesa e Livro Didático

    Directory of Open Access Journals (Sweden)

    Leticia Fraga

    2009-07-01

    Full Text Available

    Esse artigo busca identificar os papéis da lingüística no ensino de língua, identificação essa que tem como objetivo central a compreensão de como se deu a correlação entre o desenvolvimento da pesquisa e sua aplicação ao ensino. Em geral, quando se tem um tema como este, se pensa em Lingüística Aplicada e, em particular, no Ensino de Língua Estrangeira ou Língua Materna. No entanto, a perspectiva do trabalho procura relacionar a Lingüística ao desenvolvimento das bases teóricas do ensino, refletindo sobre alguns aspectos atuais da Lingüística e seu potencial, sobretudo na aplicação que dela vem sendo feita. Dessa forma, analisar-se-á nesse trabalho de que forma a proposta de ensino do sistema de escrita alfabética de um livro didático se relaciona à proposta dos Parâmetros Curriculares Nacionais em Língua Portuguesa, uma vez que esses documentos evidenciam de que forma a teoria lingüística pode influenciar o ensino de língua materna.

  17. A historicidade e o sucesso do “socialismo de mercado” chinês

    Directory of Open Access Journals (Sweden)

    Elias Jabbour

    2009-10-01

    Full Text Available Para a filosofia clássica chinesa, quando uma pessoa chega aos 60 anos chega um sinal que indica maturidade na vida terrena. Neste sentido, são altamente pertinentes a busca por respostas menos superficiais e capazes de ajudar-nos em algo que também buscamos ao trilhar o caminho brasileiro de transição ao socialismo. Serenidade, visão de processo histórico e o tato político como marca registrada daqueles que enxergam no movimento político imediato algo passivo de tratamento científico.
    Neste sentido, tendo a transição como uma categoria filosófica a ser cada vez mais degustada e trabalhada, tentarei – nestas curtas linhas – mapear o caminho do sucesso inerente ao

  1. A História do Ensino do Espanhol na década de 1980-1990 no Estado do Paraná

    Directory of Open Access Journals (Sweden)

    Jonathas de Paula Chaguri

    2011-04-01

    Full Text Available

    Este trabalho tem como objetivo apresentar os (des caminhos que levaram o estado do Paraná a um momento de reformulação em sua grade curricular, levando a saída do Espanhol como componente curricular do Colégio Estadual em Curitiba na década de 1980 e voltando a sua oferta no final da mesma década com a criação do CELEM em todo estado. Por conseguinte, o espanhol vem se solidificando em todo estado do Paraná, após a criação da Lei nº. 11.161 sancionado pelo Presidente Luiz Inácio Lula da Silva, que dispõe sobre o ensino do espanhol como componente curricular obrigatório nas escolas de ensino médio de todo o país.

  2. Violence Research from North Africa to South Asia: A Historical and Structural Overview

    Directory of Open Access Journals (Sweden)

    Jochen Hippler

    2011-07-01

    Full Text Available

    This is a historical and sociological overview of violence and violence research in and on North Africa, West Asia, and South Asia, considering only studies for a global audience. The main focus is on political violence, with a brief look at religious and communal violence, youth violence, and domestic and gendered violence. These regions have been consistently affected by political violence for many decades, the main source of which seems to be the ongoing state formation process, as well as social transformation in general. The literature on violence is dominated by international debates, at

  3. Os perigos da utopia

    Directory of Open Access Journals (Sweden)

    Larry Hufford

    2009-06-01

    Full Text Available

    A utopia pode ter um lado que eleva e um lado sinistro, mas geralmente o lado sinistro acaba destruindo o idealismo inicial. A razão para isto é que os utópicos inevitavelmente adotam uma imagem messiânica do mundo. As três revoluções messiânicas na história—a americana, a francesa e a bolchevique—foram lideradas por homens que pensavem que suas idéias eram universais. Este ensaio examina os escritos do existencialista francês Albert Camus, que argumenta que não existem valores transcendentais, ao mesmo tempo que ele não aceita o niilismo. Camus faz uma distinção entre um rebelde e um revolucionário, e conclui que uma rebelião tentará terminar com uma opressão espedífica, enquanto que uma revolução tentará criar “um novo

  4. A abordagem de Morin frente à construção do todo

    Directory of Open Access Journals (Sweden)

    Paloma Maria Santos

    2009-08-01

    Full Text Available

    O objetivo deste artigo é apresentar uma reflexão sobre a abordagem de Edgar Morin frente a construção do conhecimento. Partindo das transformações que podem ocorrer dentro de um sistema complexo, Morin discorre sobre três pressupostos relacionados a interação entre partes e todo, que irão conduzir o desenvolvimento deste trabalho.

  5. La endoscopia digestiva superior en la Atención Primaria de Salud

    Directory of Open Access Journals (Sweden)

    Marcos Félix Osorio Pagola

    2010-11-01

    Full Text Available

    .


  6. Cuando parten las ideas. Exilio y transformaciones del campo intelectual

    Directory of Open Access Journals (Sweden)

    Lorena Soler

    2008-09-01

    Full Text Available A propósito de ";El exilio intelectual en México. Notas sobre la experiencia argentina 1974-1983"; de José María Casco.

  7. Educar-se ao mundo: percepções acerca das africanidades

    Directory of Open Access Journals (Sweden)

    Paulo César Antonini de Souza

    2010-03-01

    Full Text Available

    O presente ensaio tem a intenção de apresentar algumas reflexões sobre o estudo das africanidades nas instituições de ensino. Buscando referência nas legislações que determinam essa abordagem, o texto faz um percurso histórico sobre elementos que viabilizam sua necessidade de inserção, na expectativa de que os educadores lancem um novo olhar a respeito da educação pela diversidade, assim como para os significados e sentidos do educar-se, segundo a perspectiva africana, em relação aos afro-descendentes brasileiros.

  8. Integrated geophysical measurements on a test site for detection of buried steel drums

    Directory of Open Access Journals (Sweden)

    Alessandro Settimi

    2011-04-01

    Full Text Available Geophysical methods are increasingly used to detect and locate illegal waste disposal and buried toxic steel drums. This study describes the results of a test carried out in clayey-sandy ground where 12 empty steel drums had previously been buried at 4-5 m below ground level. This test was carried out with three geophysical methods for steel-drum detection: a magnetometric survey, electrical resistivity tomography with different arrays, and a multifrequency frequency-domain electromagnetic induction survey. The data show that as partially expected, the magnetometric and electromagnetic induction surveys detected the actual steel drums buried in the subsurface, while the electrical resistivity tomography mainly detected the changes in some of the physical properties of the terrain connected with the digging operations, rather than the actual presence of the steel drums.

    Son elli yılda implantoloji alanında büyük adımlar atılmıştır. Günümüzde implantın kemik ile bağlantısı kabul edilebilir derecede başarılı olmasına rağmen inflamasyon, trombozis, fibrozis ve enfeksiyon gibi komplikasyonlar görülebilmektedir. Genetik ve doku mühendisliği alanındaki gelişmelerle birlikte ileri çalışmalara ihtiyaç duyulmaktadır. Görülen komplikasyonları en aza indirmek için implantın yerleştirildiği dokunun yanıtının istenilen düzeyde ve şekilde olması ve immün reaksiyonun düzenlenmesi gerekmektedir. Ayrıca doku mühendisliği ile implantın yerleştirilmesi için, kaybedilen alveolar kemik dokusunun yeniden oluşturulması ya da genişletilmesi mümkün hale gelmiştir.

  9. O primeiro ano de governo de Barack Obama: tempestades à toda volta

    Directory of Open Access Journals (Sweden)

    Eva Paulino Bueno

    2010-02-01

    Full Text Available O primeiro ano de Barak Obama à frente do governo americano foi um ano de grandes dificuldades, não só para ele, mas também para o seu partido democrata. Não só para os democratas, mas também para o povo americano. Não só para o povo americano, mas também para o povo iraquiano, e o povo do Afeganistão. E, por extensão, para todas as pessoas do mundo que ouviram seu discurso de aceitação do cargo, no dia 20 de janeiro de 2009. Os únicos que não sofreram, pelo que pude averiguar ouvindo rádio, lendo jornais e assistindo as notícias, foram os comentaristas republicanos, especialmente os ligados à tropa da cadeia de televisão Fox. Para eles, foi um ano de exultação.  Só não foi melhor porque o país não sofreu um ataque terrorista de

  10. The dangers of Utopia

    Directory of Open Access Journals (Sweden)

    Larry Hufford

    2009-06-01

    Full Text Available

    Utopia can have an uplifting and a dark side, but usually the dark side ends up trumping the initial idealism. The reason for this is that utopians inevitably adopt a messianic image of the world. The three messianic revolutions in history—the American, French and Bolshevik—were led by men who thought their ideas were universal. This essay examines the writings of French existentialist Albert Camus, who argues that there are no transcendental values, at the same time he does not accept nihilism. Camus makes a distinction between a rebel and a revolutionary, and concludes that a rebellion will try to end the specific oppression, whereas the revolution will try to create a “new man,” with common values throughout the world.

  11. Are you kidding me? Are you kidding me?

    Directory of Open Access Journals (Sweden)

    Rosanna Lauriola

    2010-04-01

    Full Text Available Are you kidding me?

    The presence of a picture such as the one that appears in the site (http://farm4.static.flickr.com/3252/2843406747_3c135d63d9.jpg?v=0 brings to mind both the enormous efforts made throughout many years to raise awareness about the dangers or rape, and the horrors of rape for women all over the world. To joke with such a subject is offensive both for people—men and women—who have been struggling for so long, and for the victims of this crime. People who use the subject of rape for fun cause immense pain and immense damage.

  12. Real-time monitoring of fragrance release from cotton towels by low thermal mass gas chromatography using a longitudinally modulating cryogenic system for headspace sampling and injection.

    Science.gov (United States)

    Haefliger, Olivier P; Jeckelmann, Nicolas; Ouali, Lahoussine; León, Géraldine

    2010-01-15

    An innovative headspace sampling and injection system for gas chromatography was designed using a longitudinally modulating cryogenic system mounted around the sampling loop of a two-position loop injector. The setup was hyphenated to a fast low thermal mass gas chromatograph, allowing transient concentrations of semivolatile analytes to be monitored in real time with a time resolution of 4.5 min. The performance of the instrument, and in particular its cryotrapping efficiency, was characterized using a mixture of long-chain alkanes, methyl esters, ethyl esters, and alcohols of different volatilities. The device was found to be ideally suited to the analysis of semivolatile compounds with boiling points ranging between 190 and 320 degrees C, which are typical for a majority of perfumery raw materials. The new instrument was successfully used to monitor the release of eight odorant compounds from cotton towels to which fabric softener had been applied that alternatively contained the fragrance in free form or in microencapsulated form. The analytical results, unprecedented in their level of precision and time resolution for such an application, evidenced the major impact of microencapsulation technology on the kinetics of fragrance release during the drying of the towels and on the triggering of additional fragrance release by applying mechanical stress to the fabric to rupture the microcapsule walls. PMID:20025230

  13. Zinc fate in animal husbandry systems.

    Science.gov (United States)

    Romeo, A; Vacchina, V; Legros, S; Doelsch, E

    2014-11-01

    Zinc (Zn) is considered in animal production systems as both an essential nutrient and a possible pollutant. While it is generally supplemented at low levels in animal diets, with less than 200 mg kg(-1) in complete feeds, it is under scrutiny due to potential accumulation in the environment. This explains why international regulations limit maximum supplementation levels in animal feeds in a stricter way. This article gives an overview of the current knowledge on the fate of zinc in animal production systems, from animal diets to animal wastes. Some analytical methods can be used for the quantification and qualification of Zn chemical forms: X-ray crystallography, electrospray tandem mass spectrometry, separation techniques, hyphenated techniques… Analysis of chelated forms issued from complex matrices, like hydrolysed proteins, remains difficult, and the speciation of Zn in diluted carriers (premix and feed) is a challenge. Our understanding of Zn absorption has made progress with recent research on ZnT/Zip families and metallothioneins. However, fine-tuned approaches towards the nutritional and metabolic interactions for Zn supplementation in farm conditions still require further studies. The speciation of zinc in pig manure and poultry litter has been a priority as monogastric animals are usually raised under intensive conditions and fed with high quantities of trace minerals, leading to high animal density and elevated quantities of zinc from animal wastes.

  14. Between the theatre and the street: Corporality and Peruvian immigrants in Buenos Aires Entre el teatro y la calle: Corporalidades de migrantes peruanos en Buenos Aires

    Directory of Open Access Journals (Sweden)

    Santiago Canevaro

    2008-09-01

    Full Text Available

  1. Method for the quantification of vanadyl porphyrins in fractions of crude oils by High Performance Liquid Chromatography-Flow Injection-Inductively Coupled Plasma Mass Spectrometry

    Science.gov (United States)

    Wandekoken, Flávia G.; Duyck, Christiane B.; Fonseca, Teresa C. O.; Saint'Pierre, Tatiana D.

    2016-05-01

    High performance liquid chromatography hyphenated by flow injection to inductively coupled plasma mass spectrometry (HPLC-FI-ICP-MS) was used to investigate V linked to porphyrins present in fractions of crude oil. First, the crude oil sample was submitted to fractionation by preparative liquid chromatography with UV detection, at the porphyrin Soret band wavelength (400 nm). The obtained porphyrin fractions were then separated in a 250 mm single column, in the HPLC, and eluted with different mobile phases (methanol or methanol:toluene (80:20; v:v)). The quantification of V-porphyrins in the fractions eluted from HPLC was carried out by online measuring the 51V isotope in the ICP-MS, against vanadyl octaethylporphine standard solutions (VO-OEP), prepared in the same solvent as the mobile phase, and injected post-column directly into the plasma. A 20 μg L- 1 Ge in methanol was used as internal standard for minimizing non-spectral interference, such as short-term variations due to injection. The mathematical treatment of the signal based on Fast Fourier Transform smoothing algorithm was employed to improve the precision. The concentrations of V as V-porphyrins were between 2.7 and 11 mg kg- 1 in the fractions, which were close to the total concentration of V in the porphyrin fractions of the studied crude oil.

  2. Immersed single-drop microextraction interfaced with sequential injection analysis for determination of Cr(VI) in natural waters by electrothermal-atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Single-drop microextraction (SDME) and sequential injection analysis have been hyphenated for ultratrace metal determination by Electrothermal-Atomic Absorption Spectrometry (ETAAS). The novel method was targeted on extraction of the Cr(VI)-APDC chelate and encompasses the potential of SDME as a miniaturized and virtually solvent-free preconcentration technique, the ability of sequential injection analysis to handle samples and the versatility of furnace autosamplers for introducing microliter samples in ETAAS. The variables influencing the microextraction of Cr(VI) onto an organic solvent drop, i.e., type of organic solvent, microextraction time, stirring rate of the sample solution, drop volume, immersion depth of the drop, salting-out effect, temperature of the sample, concentration of the complexing agent and pH of the sample solution were fully investigated. For a 5 and 20 min microextraction time, the preconcentration factors were 20 and 70, respectively. The detection limit was 0.02 μg/L of Cr(VI) and the repeatability expressed as relative standard deviation was 7%. The SDME-SIA-ETAAS technique was validated against BCR CRM 544 (lyophilized solution) and applied to ultrasensitive determination of Cr(VI) in natural waters

  3. Analytical methods for chemical and sensory characterization of scent-markings in large wild mammals: a review.

    Science.gov (United States)

    Soso, Simone B; Koziel, Jacek A; Johnson, Anna; Lee, Young Jin; Fairbanks, W Sue

    2014-01-01

    In conjoining the disciplines of "ethology" and "chemistry" the field of "Ethochemistry" has been instituted. Ethochemistry is an effective tool in conservation efforts of endangered species and the understanding of behavioral patterns across all species. Chemical constituents of scent-markings have an important, yet poorly understood function in territoriality, reproduction, dominance, and impact on evolutionary biology, especially in large mammals. Particular attention has recently been focused on scent-marking analysis of great cats (Kalahari leopards (Panthera pardus), puma (Puma concolor) snow leopard (Panthera uncia), African lions (Panthera leo), cheetahs (Acinonyx jubatus), and tigers (Panthera tigris)) for the purpose of conservation. Sensory analyses of scent-markings could address knowledge gaps in ethochemistry. The objective of this review is to summarize the current state-of-the art of both the chemical and sensory analyses of scent-markings in wild mammals. Specific focus is placed on sampling and sample preparation, chemical analysis, sensory analysis, and simultaneous chemical and sensory analyses. Constituents of exocrine and endocrine secretions have been most commonly studied with chromatography-based analytical separations. Odor analysis of scent-markings provides an insight into the animal's sensory perception. A limited number of articles have been published in the area of sensory characterization of scent marks. Simultaneous chemical and sensory analyses with chromatography-olfactometry hyphenation could potentially aid conservation efforts by linking perceived odor, compounds responsible for odor, and resulting behavior. PMID:24603639

  4. SIMULTANEOUS SELECTION FOR GENOTYPIC PRODUCTION, ADAPTABILITY, AND STABILITY IN CASHEW CLONES BY MIXED MODELS SELEÇÃO SIMULTÂNEA PARA PRODUÇÃO, ADAPTABILIDADE E ESTABILIDADE GENOTÍPICAS EM CLONES DE CAJUEIRO, VIA MODELOS MISTOS

    Directory of Open Access Journals (Sweden)

    José Jaime Vasconcelos Cavalcanti

    2009-01-01

    Full Text Available

    This work aimed to study the interaction between genotypes and environments, using the BLUP/REML procedure for evaluation of precocious cashew clones. The purpose of this work was to identify genotypes that simultaneously aggregate high productivity and

  5. Sulfur analysis by inductively coupled plasma-mass spectrometry: A review

    Science.gov (United States)

    Giner Martínez-Sierra, J.; Galilea San Blas, O.; Marchante Gayón, J. M.; García Alonso, J. I.

    2015-06-01

    In recent years the number of applications of sulfur (S) analysis using inductively coupled plasma mass spectrometry (ICP-MS) as detector has increased significantly. In this article we describe in some depth the application of ICP-MS for S analysis with emphasis placed on the sulfur-specific detection by hyphenated techniques such as LC, GC, CE and LA coupled on-line to ICP-MS. The different approaches available for sulfur isotope ratio measurements by ICP-MS are also detailed. Particular attention has been paid to the quantification of peptides/proteins and the analysis of metallopeptides/metalloproteins via sulfur by LC-ICP-MS. Likewise, the speciation analysis of metal-based pharmaceuticals and metallodrugs and non-metal selective detection of pharmaceuticals via S are highlighted. Labeling procedures for metabolic applications are also included. Finally, the measurement of natural variations in S isotope composition with multicollector ICP-MS instruments is also covered in this review.

  6. Technologies in quantification of plant polyphenols and its research progress%植物膳食多酚及其定量分析方法的研究进展

    Institute of Scientific and Technical Information of China (English)

    徐维盛; 杨月欣

    2013-01-01

      Plant polyphenols, with complex structures and multiple functions, are a class of plant second-ary metabolites and have been widely used in food because of its activities. This paper reviewed the kinds of plant polyphenols such as tea polyphenol, grape polyphenol, apple polyphenol, pomegranate polyphenol, and algae polyphenols, and the detection methods such as high pressure liquid chromatography, gas chromatogra-phy, high performance capillary electrophoresis, infrared spectroscopy, nuclear magnetic resonance spectros-copy, and some hyphenated techniques to provide a reference for the further study.%  植物多酚是一种植物次生代谢物,其结构多样,具有多种生物活性。本文对近年来研究较多的植物多酚(茶多酚、葡萄多酚、苹果多酚、石榴多酚、海藻多酚)及其定量分析方法(高压液相色谱法、气相色谱法、毛细管电泳法,红外光谱法、核磁共振波谱法及各种联用技术)进行了综述,以期为植物多酚的后续研究提供参考。

  7. HPTLC-aptastaining - Innovative protein detection system for high-performance thin-layer chromatography

    Science.gov (United States)

    Morschheuser, Lena; Wessels, Hauke; Pille, Christina; Fischer, Judith; Hünniger, Tim; Fischer, Markus; Paschke-Kratzin, Angelika; Rohn, Sascha

    2016-05-01

    Protein analysis using high-performance thin-layer chromatography (HPTLC) is not commonly used but can complement traditional electrophoretic and mass spectrometric approaches in a unique way. Due to various detection protocols and possibilities for hyphenation, HPTLC protein analysis is a promising alternative for e.g., investigating posttranslational modifications. This study exemplarily focused on the investigation of lysozyme, an enzyme which is occurring in eggs and technologically added to foods and beverages such as wine. The detection of lysozyme is mandatory, as it might trigger allergenic reactions in sensitive individuals. To underline the advantages of HPTLC in protein analysis, the development of innovative, highly specific staining protocols leads to improved sensitivity for protein detection on HPTLC plates in comparison to universal protein derivatization reagents. This study aimed at developing a detection methodology for HPTLC separated proteins using aptamers. Due to their affinity and specificity towards a wide range of targets, an aptamer based staining procedure on HPTLC (HPTLC-aptastaining) will enable manifold analytical possibilities. Besides the proof of its applicability for the very first time, (i) aptamer-based staining of proteins is applicable on different stationary phase materials and (ii) furthermore, it can be used as an approach for a semi-quantitative estimation of protein concentrations.

  8. Determination of biogenic amines in wines by pre-column derivatization and high-performance liquid chromatography coupled to mass spectrometry.

    Science.gov (United States)

    García-Villar, Natividad; Hernández-Cassou, Santiago; Saurina, Javier

    2009-09-01

    A new HPLC method for determining biogenic amines in wines is developed. This method is based on pre-column amine derivatization, further separation of derivatives and on-line hyphenation of HPLC to atmospheric pressure chemical ionization mass spectrometry (APCI-MS). Biogenic amines have been derivatized with 1,2-naphthoquinone-4-sulfonate at 65 degrees C and pH 9.2 for 5 min. The separation of derivatives has been accomplished in a C(18) analytical column using an elution gradient based on increasing the percentage of methanol. Derivatives have been ionized in positive mode and detected by selected ion monitoring. The operating conditions of the APCI-MS system (voltages, temperatures and gases) have been thoroughly optimized to obtain the maximum sensitivity for all analytes. In the selected conditions, APCI-MS spectra display little fragmentation and good signal-to-noise ratio. Depending on the amine characteristics, the main spectral peaks are due to mono- and di-derivative products. Figures of merit of the method have been established under the selected conditions using red wine samples. Recoveries ranging from 94% to 106% have been obtained which prove excellent accuracy of the method in the determination of histamine, putrescine, cadaverine, tryptamine, phenylethylamine, tyramine and serotonin in red wines. The proposed method has been applied to the analysis of commercial wines from different Spanish regions.

  9. Chemical Characterization and in Vitro Antibacterial Activity of Myrcianthes hallii (O. Berg McVaugh (Myrtaceae, a Traditional Plant Growing in Ecuador

    Directory of Open Access Journals (Sweden)

    Patricia Chavez Carvajal

    2016-06-01

    Full Text Available Myrcianthes hallii (O. Berg McVaugh (Myrtaceae is a plant native to Ecuador, traditionally used for its antiseptic properties. The composition of the hydro-methanolic extract of this plant was determined by submitting it to ultra-high performance liquid chromatography (UHPLC hyphenated to heated-electrospray ionization mass spectrometry and UV detection. The presence of antimicrobial components prompted us to test the extract against methicillin-resistant and methicillin-susceptible Staphylococcus aureus, multidrug-resistant and susceptible Escherichia coli, Pseudomonas aeruginosa, Enterococcus spp. and Streptococcus pyogenes strains. The chromatographic analysis led to the identification of 38 compounds, including polyphenols and organic acids, and represents the first chemical characterization of this plant. The extract showed modest antibacterial activity against all tested bacteria, with the exception of E. coli which was found to be less sensitive. Whilst methicillin-resistant strains usually display resistance to several drugs, no relevant differences were observed between methicillin-susceptible and resistant strains. Considering its long-standing use in folk medicine, which suggests the relative safety of the plant, and the presence of many known antibacterial polyphenolic compounds responsible for its antibacterial activity, the results show that M. hallii extract could be used as a potential new antiseptic agent. Moreover, new anti-infective biomaterials and nanomaterials could be designed through the incorporation of M. hallii polyphenols. This prospective biomedical application is also discussed.

  10. 铀在植物-微生物共生体系满江红体内的分布%Distribution of Uranium in the Plant_microbe Symbiotic System_Azolla Imbircata

    Institute of Scientific and Technical Information of China (English)

    胡南; 丁德馨; 潘长春; 胡劲松; 李乐; 李广悦; 王永东; 郑济芳

    2014-01-01

    采用扫描电镜( SEM)和能谱( EDS)联用分析技术,研究了铀在植物—微生物共生体系满江红中的分布,结果发现,铀在蕨类植物满江红和微生物满江红鱼腥藻中均有分布,满江红鱼腥藻中铀含量略高于蕨类植物满江红,表明了蕨类植物满江红和微生物满江红鱼腥藻都参与了去除水体中铀的过程。%The distribution of uranium in the plant_microbe symbiotic system_Azolla imbir_cata was analyzed by scanning electron microscope( SEM) and energy dispersive spectrom_eter( EDS ) hyphenated technique. The results showed that uranium distributed in both fern_Azolla imbricata and microbe_Anabena azollae. The content of uranium in Anabena azollae was slightly higher than that in Azolla imbricata. The fern_Azolla imbricata and mi_crobe_Anabena azollae had a synergistic effect on the process of removing uranium from the water.

  11. Recent trends in the impurity profile of pharmaceuticals

    Directory of Open Access Journals (Sweden)

    Kavita Pilaniya

    2010-01-01

    Full Text Available Various regulatory authorities such as the International Conference on Harmonization (ICH, the United States Food and Drug administration (FDA, and the Canadian Drug and Health Agency (CDHA are emphasizing on the purity requirements and the identification of impurities in Active Pharmaceutical Ingredients (APIs. The various sources of impurity in pharmaceutical products are - reagents, heavy metals, ligands, catalysts, other materials like filter aids, charcoal, and the like, degraded end products obtained during \\ after manufacturing of bulk drugs from hydrolysis, photolytic cleavage, oxidative degradation, decarboxylation, enantiomeric impurity, and so on. The different pharmacopoeias such as the British Pharmacopoeia, United State Pharmacopoeia, and Indian Pharmacopoeia are slowly incorporating limits to allowable levels of impurities present in APIs or formulations. Various methods are used to isolate and characterize impurities in pharmaceuticals, such as, capillary electrophoresis, electron paramagnetic resonance, gas-liquid chromatography, gravimetric analysis, high performance liquid chromatography, solid-phase extraction methods, liquid-liquid extraction method, Ultraviolet Spectrometry, infrared spectroscopy, supercritical fluid extraction column chromatography, mass spectrometry, Nuclear magnetic resonance (NMR spectroscopy, and RAMAN spectroscopy. Among all hyphenated techniques, the most exploited techniques for impurity profiling of drugs are Liquid Chromatography (LC-Mass Spectroscopy (MS, LC-NMR, LC-NMR-MS, GC-MS, and LC-MS. This reveals the need and scope of impurity profiling of drugs in pharmaceutical research.

  12. Handheld spectrometers: the state of the art

    Science.gov (United States)

    Crocombe, Richard A.

    2013-05-01

    "Small" spectrometers fall into three broad classes: small versions of laboratory instruments, providing data, subsequently processed on a PC; dedicated analyzers, providing actionable information to an individual operator; and process analyzers, providing quantitative or semi-quantitative information to a process controller. The emphasis of this paper is on handheld dedicated analyzers. Many spectrometers have historically been large, possible fragile, expensive and complicated to use. The challenge over the last dozen years, as instruments have moved into the field, has been to make spectrometers smaller, affordable, rugged, easy-to-use, but most of all capable of delivering actionable results. Actionable results can dramatically improve the efficiency of a testing process and transform the way business is done. There are several keys to this handheld spectrometer revolution. Consumer electronics has given us powerful mobile platforms, compact batteries, clearly visible displays, new user interfaces, etc., while telecomm has revolutionized miniature optics, sources and detectors. While these technologies enable miniature spectrometers themselves, actionable information has demanded the development of rugged algorithms for material confirmation, unknown identification, mixture analysis and detection of suspicious materials in unknown matrices. These algorithms are far more sophisticated than the `correlation' or `dot-product' methods commonly used in benchtop instruments. Finally, continuing consumer electronics advances now enable many more technologies to be incorporated into handheld spectrometers, including Bluetooth, wireless, WiFi, GPS, cameras and bar code readers, and the continued size shrinkage of spectrometer `engines' leads to the prospect of dual technology or `hyphenated' handheld instruments.

  13. The use of laser-induced fluorescence or ultraviolet detectors for sensitive and selective analysis of tobramycin or erythropoietin in complex samples

    Science.gov (United States)

    Ahmed, Hytham M.; Ebeid, Wael B.

    2015-05-01

    Complex samples analysis is a challenge in pharmaceutical and biopharmaceutical analysis. In this work, tobramycin (TOB) analysis in human urine samples and recombinant human erythropoietin (rhEPO) analysis in the presence of similar protein were selected as representative examples of such samples analysis. Assays of TOB in urine samples are difficult because of poor detectability. Therefore laser induced fluorescence detector (LIF) was combined with a separation technique, micellar electrokinetic chromatography (MEKC), to determine TOB through derivatization with fluorescein isothiocyanate (FITC). Borate was used as background electrolyte (BGE) with negative-charged mixed micelles as additive. The method was successively applied to urine samples. The LOD and LOQ for Tobramycin in urine were 90 and 200 ng/ml respectively and recovery was >98% (n = 5). All urine samples were analyzed by direct injection without sample pre-treatment. Another use of hyphenated analytical technique, capillary zone electrophoresis (CZE) connected to ultraviolet (UV) detector was also used for sensitive analysis of rhEPO at low levels (2000 IU) in the presence of large amount of human serum albumin (HSA). Analysis of rhEPO was achieved by the use of the electrokinetic injection (EI) with discontinuous buffers. Phosphate buffer was used as BGE with metal ions as additive. The proposed method can be used for the estimation of large number of quality control rhEPO samples in a short period.

  14. Microfabrication, separations, and detection by mass spectrometry on ultrathin-layer chromatography plates prepared via the low-pressure chemical vapor deposition of silicon nitride onto carbon nanotube templates.

    Science.gov (United States)

    Kanyal, Supriya S; Häbe, Tim T; Cushman, Cody V; Dhunna, Manan; Roychowdhury, Tuhin; Farnsworth, Paul B; Morlock, Gertrud E; Linford, Matthew R

    2015-07-24

    Microfabrication of ultrathin-layer chromatography (UTLC) plates via conformal deposition of silicon nitride by low-pressure chemical vapor deposition onto patterned carbon nanotube (CNT) scaffolds was demonstrated. After removal of the CNTs and hydroxylation, the resulting UTLC phase showed no expansion or distortion of their microfeatures and the absence/reduction of remaining nitrogenic species. Developing time of a mixture of lipophilic dyes on this UTLC plates was 86% shorter than on high-performance thin-layer chromatography (HPTLC) plates. A water-soluble food dye mixture was also separated resulting in low band broadening and reduced developing time compared to HPTLC. For the latter example, mobile phase optimization on a single UTLC plate consisted of 14 developments with different mobile phases, each preceded by a plate prewashing step. The same plate was again reused for additional 11 separations under varying conditions resulting in a development procedure with a mean separation efficiency of 233,000theoretical plates/m and a reduced mobile phase consumption of only 400μL. This repeated use proved the physical robustness of the ultrathin layer and its resistance to damage. The layer was highly suited for hyphenation to ambient mass spectrometry, including desorption electrospray ionization (DESI) mass spectrometry imaging and direct analysis in real time (DART) mass spectrometry.

  15. Electrospun nanofiber layers with incorporated photoluminescence indicator for chromatography and detection of ultraviolet-active compounds.

    Science.gov (United States)

    Kampalanonwat, Pimolpun; Supaphol, Pitt; Morlock, Gertrud E

    2013-07-19

    For the first time, electrospun nanofiber phases were fabricated with manganese-activated zinc silicate as photoluminescent indicator (UV254) to transfer and enlarge its application to the field of UV-active compounds. By integration of such an indicator, UV-active compounds got visible on the chromatogram. The separation of 7 preservatives and a beverage sample were studied on the novel luminescent polyacrylonitrile layers. The mat thickness and mean fiber diameters were calculated for additions of different UV254 indicator concentrations. The separation efficiency on the photoluminescent layers was characterized by comparison to HPTLC layers and calculation of the plate numbers and resolutions. Some benefits were the reduction in migration distance (3cm), migration time (12min), analyte (10-nL volumes) and mobile phase volumes (1mL). As ultrathin stationary phase, such layers are suited for their integration into the Office Chromatography concept. For the first time, electrospun nanofiber layers were hyphenated with mass spectrometry and the confirmation of compounds was successfully performed using the elution-head based TLC-MS Interface.

  16. Determination of Noncovalent Binding Using a Continuous Stirred Tank Reactor as a Flow Injection Device Coupled to Electrospray Ionization Mass Spectrometry

    Science.gov (United States)

    Santos, Inês C.; Waybright, Veronica B.; Fan, Hui; Ramirez, Sabra; Mesquita, Raquel B. R.; Rangel, António O. S. S.; Fryčák, Petr; Schug, Kevin A.

    2015-07-01

    Described is a new method based on the concept of controlled band dispersion, achieved by hyphenating flow injection analysis with ESI-MS for noncovalent binding determinations. A continuous stirred tank reactor (CSTR) was used as a FIA device for exponential dilution of an equimolar host-guest solution over time. The data obtained was treated for the noncovalent binding determination using an equimolar binding model. Dissociation constants between vancomycin and Ac-Lys(Ac)-Ala-Ala-OH peptide stereoisomers were determined using both the positive and negative ionization modes. The results obtained for Ac- L-Lys(Ac)- D-Ala- D-Ala (a model for a Gram-positive bacterial cell wall) binding were in reasonable agreement with literature values made by other mass spectrometry binding determination techniques. Also, the developed method allowed the determination of dissociation constants for vancomycin with Ac- L-Lys(Ac)- D-Ala- L-Ala, Ac- L-Lys(Ac)- L-Ala- D-Ala, and Ac- L-Lys(Ac)- L-Ala- L-Ala. Although some differences in measured binding affinities were noted using different ionization modes, the results of each determination were generally consistent. Differences are likely attributable to the influence of a pseudo-physiological ammonium acetate buffer solution on the formation of positively- and negatively-charged ionic complexes.

  17. Assessment of dietary exposure and effect in humans: The role of NMR.

    Science.gov (United States)

    van Duynhoven, John P M; Jacobs, Doris M

    2016-08-01

    In human nutritional science progress has always depended strongly on analytical measurements for establishing relationships between diet and health. This field has undergone significant changes as a result of the development of NMR and mass spectrometry methods for large scale detection, identification and quantification of metabolites in body fluids. This has allowed systematic studies of the metabolic fingerprints that biological processes leave behind, and has become the research field of metabolomics. As a metabolic profiling technique, NMR is at its best when its unbiased nature, linearity and reproducibility are exploited in well-controlled nutritional intervention and cross-sectional population screening studies. Although its sensitivity is less good than that of mass spectrometry, NMR has maintained a strong position in metabolomics through implementation of standardisation protocols, hyphenation with mass spectrometry and chromatographic techniques, accurate quantification and spectral deconvolution approaches, and high-throughput automation. Thus, NMR-based metabolomics has contributed uniquely to new insights into dietary exposure, in particular by unravelling the metabolic fates of phytochemicals and the discovery of dietary intake markers. NMR profiling has also contributed to the understanding of the subtle effects of diet on central metabolism and lipoprotein metabolism. In order to hold its ground in nutritional metabolomics, NMR will need to step up its performance in sensitivity and resolution; the most promising routes forward are the analytical use of dynamic nuclear polarisation and developments in microcoil construction and automated fractionation. PMID:27573181

  18. Online coupling of pure O2 thermo-optical methods - 14C AMS for source apportionment of carbonaceous aerosols

    Science.gov (United States)

    Agrios, Konstantinos; Salazar, Gary; Zhang, Yan-Lin; Uglietti, Chiara; Battaglia, Michael; Luginbühl, Marc; Ciobanu, Viorela Gabriela; Vonwiller, Matthias; Szidat, Sönke

    2015-10-01

    This paper reports on novel separation methods developed for the direct determination of 14C in organic carbon (OC) and elemental carbon (EC), two sub-fractions of total carbon (TC) of atmospheric air particulate matter. Until recently, separation of OC and EC has been performed off-line by manual and time-consuming techniques that relied on the collection of massive CO2 fractions. We present here two on-line hyphenated techniques between a Sunset OC/EC analyzer and a MICADAS (MIni radioCArbon DAting System) accelerator mass spectrometer (AMS) equipped with a gas ion source. The first implementation facilitates the direct measurement in the low sample size range (<10 μg C) with high throughput on a routine basis, while the second explores the potential for a continuous-flow real-time CO2 gas feed into the ion source. The performance achieved with reference materials and real atmospheric samples will be discussed to draw conclusions on the improvement offered in the field of 14C aerosol source apportionment.

  19. Profiling the substitution pattern of xyloglucan derivatives by integrated enzymatic hydrolysis, hydrophilic-interaction liquid chromatography and mass spectrometry.

    Science.gov (United States)

    Liu, Jun; Kisonen, Victor; Willför, Stefan; Xu, Chunlin; Vilaplana, Francisco

    2016-09-01

    Plant polysaccharides constitute arguably the most complex family of biomacromolecules in terms of the stereochemistry and regiochemistry of their intramolecular linkages. The chemical modification of such polysaccharides introduces an additional level of complexity for structural determinations. We have developed an integrated analytical procedure combining selective enzymatic hydrolysis, hydrophilic interaction liquid chromatography (HILIC), and mass spectrometry (MS) to describe the substitution pattern of xyloglucan (XyG) and its chemo-enzymatic derivatives (cationic, anionic, and benzyl aminated). Enzymatic hydrolysis of XyG derivatives by a xyloglucan-specific endoglucanase (XEG) generates oligosaccharides amenable for mass spectrometric identification with distinct structures, based on enzymatic substrate recognition and hydrolytic pattern. Matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry (MALDI-ToF-MS) and electrospray ionisation mass spectrometry (ESI-MS) offer qualitative mass profiling of the chemical derivatives. Separation and identification of the complex oligosaccharide profiles released by enzymatic hydrolysis is achieved by hyphenation of hydrophilic interaction liquid chromatography with mass spectrometry (HILIC-ESI-MS). Further fragmentation by tandem mass spectrometry (ESI-MS/MS) in positive mode enables the structural sequencing of modified XyG oligosaccharides and the identification of the substituent position without further derivatisation. This integrated approach can be used to obtain semi-quantitative information of the substitution pattern of hemicellulose derivatives, with fundamental implications for their modification mechanisms and performance. PMID:27524300

  20. THEORETICAL FOUNDATIONS OF COMPOSING A REFERENCE BOOK OF REGIONAL TOPONYMS

    Directory of Open Access Journals (Sweden)

    Ilyin Dmitriy Yuryevich

    2014-09-01

    Full Text Available The article deals with the linguistic issues of composing a reference book of regional toponyms – a genre that requires special consideration in national lexicography. The assortment of these issues gave the possibility to carry out complex description of regional toponyms on the basis of semantic, functional, and orpthologuos criteria that let unify the names of Volgograd region settlements that are registered in various documents. The significance of the composed reference book is determined by several factors – the presence of local subsystems of geographical names in Russian toponymy; the inconsistency of current orthography norms on using capital letter in compound proprius names and fused-with-hyphen spelling of toponyms and off-toponym derivations; the lack of linguistically justified explanation of peculiarities of grammatical norms in the field of proper names use. The reference book of regional toponyms is based on the object description (toponymic vocabulary, principles of lexical units selection (description of spelling and grammatical properties of toponyms, encyclopedic information, the glossary (full list of toponyms of Volgograd region, typical article. The articles in the reference book are arranged in lexicographical zones with grammatical and semantic markers, lexicographical illustrations, other lexicographical labels, word etymology including. The reference book on Volgograd region toponymy is addressed to executive and administration authorities, journalists, regional ethnographers.

  1. Analytical developments for the speciation of uranium in zebra fish (Danio rerio) gills after exposure

    International Nuclear Information System (INIS)

    The objective of this thesis is to study the cellular compartmentalization and the chelation of uranium (U) by cytosolic proteins of gill cells of the zebra fish (Danio rerio, model specie in aquatic toxicology) under different direct exposure conditions (chronic vs. acute, 20 and 250 μg.L-1). This study required the development of hyphenated techniques (SEC, IEF off-gel, RP-UHPLC for the separation, ICP-SFMS, ESI-FTMS/MS for the detection) with the main challenges of maintaining the non-covalent U-biomolecule interactions and enhancing sensitivity for the analysis of environmentally relevant samples. After extraction, 24% to 32% of the total U detected in the gills were present in the cytosolic fraction, in which the U distribution on the biomolecules (as a function of their MW and pI) varied depending on the exposure level. Finally, U target biomolecules mapping allowed us (i) to highlight a particular affinity of U for acidic and/or P-containing proteins and (ii) to identify 24 protein candidates for U binding. (author)

  2. DEVELOPMENT OF Annona crassiflora Mart. (ARATICUM SEEDLINGS IN SUBSTRATA WITH SUGAR CANE BAGASSE ASH DESENVOLVIMENTO DE MUDAS DE Annona crassiflora Mart. (ARATICUM EM SUBSTRATOS COM CINZA DE BAGAÇO DE CANA

    Directory of Open Access Journals (Sweden)

    Andréia Luiza Salgado

    2009-01-01

    Full Text Available

    The effect of five growing media, in different proportions of subsoil, limestone, and sugar cane bagasse ash, in the height, stem diameter, and fresh and dry weight of the aerial part and roots of araticum seedlings (Annona crassiflora Mart. was analyzed. The five growing media were

  3. Sol-gel microextraction phases for sample preconcentration in chromatographic analysis.

    Science.gov (United States)

    Segro, Scott S; Tran, Minh Phuong; Kesani, Sheshanka; Alhendal, Abdullah; Turner, Erica B

    2010-10-01

    Sol-gel technology provides a simple and reliable method for solid-phase microextraction (SPME) fiber preparation through in situ creation of surface-bonded organic-inorganic hybrid coatings characterized by enhanced thermal stability and solvent-resistance properties that are important for the coupling of SPME with GC and HPLC, respectively. The sol-gel coating technology has led to the development of an extensive array of sol-gel sorbent coatings for SPME. In this article, sol-gel microextraction coatings are reviewed, with particular attention on their synthesis, characterization, and applications in conjunction with GC and HPLC analyses. In addition, the development of sol-gel-coated stir bars, their inherent advantages, and applications are discussed. Next, the development and applications of sol-gel capillary microextraction (CME) in hyphenation with GC and HPLC is extensively reviewed. The newly emerging germania- and titania-based sol-gel microextraction phases look promising, especially in terms of pH and hot solvent stability. Finally, sol-gel monolithic beds for CME are reviewed. Such monolithic beds are in a position to greatly improve the extracting capabilities and enhanced sensitivity in CME.

  4. Aspectos toxicológicos e inmunológicos del veneno del escorpión Tityus pachyurus

    Directory of Open Access Journals (Sweden)

    Rafael Valderrama

    2001-04-01

    Full Text Available

    pi*) 378 and 384 nm (n-->pi*)] and IR (1428, 1266, 1249, 1206, 1044, 822, 750, 546 and 454 cm(-1)) spectroscopy. The DSC clearly showed the sublimation of N2O5 at 32 degrees C. The nitration studies on 2,6,8,12-tetraacetylhexaaza tetracyclo[5,5,0,0(3,11)0(5,9)]dodecane (TAIW) proved its viability in 2,4,6,8,10,12-hexanitro-2,4,6,8(10,12))-hexaazatetracyclo [5,5,0,0(3,11)0(5,9)]dodecane (CL-20) synthesis. The synthesized CL-20 and its precursors have also been subjected to hyphenated TG-FTIR studies to understand decomposition pattern. PMID:15979786

  5. Analytical methods for the endocrine disruptor compounds determination in environmental water samples.

    Science.gov (United States)

    Locatelli, Marcello; Sciascia, Francesco; Cifelli, Roberta; Malatesta, Luciano; Bruni, Pantaleone; Croce, Fausto

    2016-02-19

    The potential risk of exposure to different xenobiotics, which can modulate the endocrine system and represent a treat for the wellness of an increasing number of people, has recently drawn the attention of international environmental and health agencies. Several agents, characterized by structural diversity, may interfer with the normal endocrine functions that regulate cell growth, homeostasis and development. Substances such as pesticides, herbicides, plasticizers, metals, etc. having endocrine activity (EDCs) are used in agriculture and industry and are also used as drugs for humans and animals. A difficulty in the analytical determination of these substances is the complexity of the matrix in which they are present. In fact, the samples most frequently analyzed consist of groundwater and surface water, including influent and effluent of wastewater treatment plants and drinking water. In this review, several sample pretreatment protocols, assays and different instrumental techniques recently used in the EDCs determination have been considered. This review concludes with a paragraph in which the most recent hyphenated-instrument techniques are treated, highlighting their sensitivity and selectivity for the analyses of environmental water samples.

  6. Dual ultrasonic-assisted dispersive liquid-liquid microextraction coupled with microwave-assisted derivatization for simultaneous determination of 20(S)-protopanaxadiol and 20(S)-protopanaxatriol by ultra high performance liquid chromatography-tandem mass spectrometry.

    Science.gov (United States)

    Zhao, Xian-En; Lv, Tao; Zhu, Shuyun; Qu, Fei; Chen, Guang; He, Yongrui; Wei, Na; Li, Guoliang; Xia, Lian; Sun, Zhiwei; Zhang, Shijuan; You, Jinmao; Liu, Shu; Liu, Zhiqiang; Sun, Jing; Liu, Shuying

    2016-03-11

    This paper, for the first time, reported a speedy hyphenated technique of low toxic dual ultrasonic-assisted dispersive liquid-liquid microextraction (dual-UADLLME) coupled with microwave-assisted derivatization (MAD) for the simultaneous determination of 20(S)-protopanaxadiol (PPD) and 20(S)-protopanaxatriol (PPT). The developed method was based on ultra high performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) detection using multiple-reaction monitoring (MRM) mode. A mass spectrometry sensitizing reagent, 4'-carboxy-substituted rosamine (CSR) with high reaction activity and ionization efficiency was synthesized and firstly used as derivatization reagent. Parameters of dual-UADLLME, MAD and UHPLC-MS/MS conditions were all optimized in detail. Low toxic brominated solvents were used as extractant instead of traditional chlorinated solvents. Satisfactory linearity, recovery, repeatability, accuracy and precision, absence of matrix effect and extremely low limits of detection (LODs, 0.010 and 0.015ng/mL for PPD and PPT, respectively) were achieved. The main advantages were rapid, sensitive and environmentally friendly, and exhibited high selectivity, accuracy and good matrix effect results. The proposed method was successfully applied to pharmacokinetics of PPD and PPT in rat plasma. PMID:26877173

  7. Extracting numeric measurements and temporal coordinates from Japanese radiological reports

    Science.gov (United States)

    Imai, Takeshi; Onogi, Yuzo

    2004-04-01

    Medical records are written mainly, in natural language. The focus of this study is narrative radiological reports written in natural Japanese. These reports cannot be used for advanced retrieval, data mining, and so on, unless they are stored, using a structured format such as DICOM-SR. The goal is to structure narrative reports progressively, using natural language processing (NLP). Structure has many different levels, for example, DICOM-SR has three established levels -- basic text, enhanced and comprehensive. At the enhanced level, it is necessary to use numerical measurements and spatial & temporal coordinates. In this study, the wording used in the reports was first standardized, dictionaries were organized, and morphological analysis performed. Next, numerical measurements and temporal coordinates were extracted, and the objects to which they referred, analyzed. 10,000 CT and MR reports were separated into 82,122 sentences, and 34,269 of the 36,444 numerical descriptions were tagged. Periods, slashes, hyphens, and parentheses are ambiguously used in the description of enumerated lists, dates, image numbers, and anatomical names, as well as at the end of sentences; to resolve this ambiguity, descriptions were processed, according to the order -- date, size, unit, enumerated list, and abbreviation -- then, the tagged reports were separated into sentences.

  8. Characterization and Quantification of Compounds in the Hydroalcoholic Extract of the Leaves from Terminalia catappa Linn. (Combretaceae and Their Mutagenic Activity

    Directory of Open Access Journals (Sweden)

    Francisco José Mininel

    2014-01-01

    Full Text Available Terminalia is a genus of Combretaceous plants widely distributed in tropical and subtropical regions. Thus, the aim of this study was to quantify the majority compounds of the hydroalcoholic extract (7 : 3, v/v of the leaves from T. catappa by HPLC-PDA, chemically characterize by hyphenated techniques (HPLC-ESI-IT-MSn and NMR, and evaluate its mutagenic activity by the Salmonella/microsome assay on S. typhimurium strains TA98, TA97a, TA100, and TA102. The quantification of analytes was performed using an external calibration standard. Punicalagin is the most abundant polyphenol found in the leaves. The presence of this compound as a mixture of anomers was confirmed using HPLC-PDA and 1H and 13C NMR. Mutagenic activity was observed in strains TA100 and TA97a. As the extract is a complex mixture of punicalagin, its derivatives, and several other compounds, the observed mutagenicity may be explained in part by possible synergistic interaction between the compounds present in the extract. These studies show that mutagenic activity of T. catappa in the Ames test can only be observed when measured at high concentrations. However, considering the mutagenic effects observed for T. catappa, this plant should be used cautiously for medicinal purposes.

  1. Introduction to engineering electromagnetics

    CERN Document Server

    Lee, Yeon Ho

    2013-01-01

    This text provides students with the missing link that can help them master the basic principles of electromagnetics. The concept of vector fields is introduced by starting with clear definitions of position, distance, and base vectors. The symmetries of typical configurations are discussed in detail, including cylindrical, spherical, translational, and two-fold rotational symmetries. To avoid serious confusion between symbols with two indices, the text adopts a new notation: a letter with subscript 1-2 for the work done in moving a unit charge from point 2 to point 1, in which the subscript 1-2 mimics the difference in potentials, while the hyphen implies a sense of backward direction, from 2 to 1. This text includes 300 figures in which real data are drawn to scale. Many figures provide a three-dimensional view. Each subsection includes a number of examples that are solved by examining rigorous approaches in steps. Each subsection ends with straightforward exercises and answers through which students can c...

  2. Analytical Methods for Chemical and Sensory Characterization of Scent-Markings in Large Wild Mammals: A Review

    Directory of Open Access Journals (Sweden)

    Simone B. Soso

    2014-03-01

    Full Text Available In conjoining the disciplines of “ethology” and “chemistry” the field of “Ethochemistry” has been instituted. Ethochemistry is an effective tool in conservation efforts of endangered species and the understanding of behavioral patterns across all species. Chemical constituents of scent-markings have an important, yet poorly understood function in territoriality, reproduction, dominance, and impact on evolutionary biology, especially in large mammals. Particular attention has recently been focused on scent-marking analysis of great cats (Kalahari leopards (Panthera pardus, puma (Puma concolor snow leopard (Panthera uncia, African lions (Panthera leo, cheetahs (Acinonyx jubatus, and tigers (Panthera tigris for the purpose of conservation. Sensory analyses of scent-markings could address knowledge gaps in ethochemistry. The objective of this review is to summarize the current state-of-the art of both the chemical and sensory analyses of scent-markings in wild mammals. Specific focus is placed on sampling and sample preparation, chemical analysis, sensory analysis, and simultaneous chemical and sensory analyses. Constituents of exocrine and endocrine secretions have been most commonly studied with chromatography-based analytical separations. Odor analysis of scent-markings provides an insight into the animal’s sensory perception. A limited number of articles have been published in the area of sensory characterization of scent marks. Simultaneous chemical and sensory analyses with chromatography-olfactometry hyphenation could potentially aid conservation efforts by linking perceived odor, compounds responsible for odor, and resulting behavior.

  3. Separation of maleic anhydride grafted polypropylene using multidimensional high-temperature liquid chromatography.

    Science.gov (United States)

    Prabhu, K N; Macko, T; Brüll, R; Remerie, K; Tacx, J; Garg, P; Ginzburg, A

    2016-04-01

    Functionalization addresses a property gap of polyolefins and opens new perspectives due to improved surface properties in applications like composites (e.g., glass fiber reinforced polypropylene) and anti-corrosive coatings for metals. Various techniques have been developed to characterize functionalized polyolefins, yet no analytical approach addressing their chemical heterogeneity exists. Using High Temperature Size Exclusion Chromatography (HT-SEC) coupled to infrared spectroscopy we could show for two model samples of polypropylene grafted maleic anhydride (PP-g-MA), differing in their nominal MA content, that the grafting density increases with decreasing molar mass. Crystallization Analysis Fractionation (CRYSTAF) does not enable to separate these samples according to their composition to the extent required. Yet, when using High Temperature High Performance Liquid Chromatography (HT-HPLC), with either silica gel or Mica as stationary phase and a gradient mobile phase, a deformulation into a grafted and a non-grafted fraction could be achieved. This was confirmed by analyzing the eluted fractions by infrared spectroscopy. Hyphenating the separation according to composition with a separation according to molar mass (HT-HPLC x HT-SEC) enabled for the first time to reveal the bivariate distribution of PP-g-MA with regard to the molar mass and composition. Using on-line infrared detection quantitative information on the compositional and molar mass parameters of the individual fractions could be obtained. PMID:26961914

  4. Real Time Monitoring of Containerless Microreactions in Acoustically Levitated Droplets via Ambient Ionization Mass Spectrometry.

    Science.gov (United States)

    Crawford, Elizabeth A; Esen, Cemal; Volmer, Dietrich A

    2016-09-01

    Direct in-droplet (in stillo) microreaction monitoring using acoustically levitated micro droplets has been achieved by combining acoustic (ultrasonic) levitation for the first time with real time ambient tandem mass spectrometry (MS/MS). The acoustic levitation and inherent mixing of microliter volumes of reactants (3 μL droplets), yielding total reaction volumes of 6 μL, supported monitoring the acid-catalyzed degradation reaction of erythromycin A. This reaction was chosen to demonstrate the proof-of-principle of directly monitoring in stillo microreactions via hyphenated acoustic levitation and ambient ionization mass spectrometry. The microreactions took place completely in stillo over 30, 60, and 120 s within the containerless stable central pressure node of an acoustic levitator, thus readily promoting reaction miniaturization. For the evaluation of the miniaturized in stillo reactions, the degradation reactions were also carried out in vials (in vitro) with a total reaction volume of 400 μL. The reacted in vitro mixtures (6 μL total) were similarly introduced into the acoustic levitator prior to ambient ionization MS/MS analysis. The in stillo miniaturized reactions provided immediate real-time snap-shots of the degradation process for more accurate reaction monitoring and used a fraction of the reactants, while the larger scale in vitro reactions only yielded general reaction information. PMID:27505037

  5. Determination of tellurium by hydride generation with in situ trapping flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Matusiewicz, H.; Krawczyk, M. [Politechn Poznanska, Poznan (Poland)

    2007-03-15

    The analytical performance of coupled hydride generation - integrated atom trap (HG-IAT) atomizer flame atomic absorption spectrometry (FAAS) system was evaluated for determination of Te in reference material (GBW 07302 Stream Sediment), coal fly ash and garlic. Tellurium, using formation of H{sub 2}Te vapors, is atomized in air-acetylene flame-heated IAT. A new design HG-IAT-FAAS hyphenated technique that would exceed the operational capabilities of existing arrangernents (a water-cooled single silica tube, double-slotted quartz tube or an 'integrated trap') was investigated. An improvement in detection limit was achieved compared with using either of the above atom trapping techniques separately. The concentration detection limit, defined as 3 times the blank standard deviation (3{sigma}), was 0.9 ng mL{sup -1} for Te. For a 2 min in situ preconcentration time (sample volume of 2 mL), sensitivity enhancement compared to flame AAS, was 222 fold, using the hydride generation atom trapping technique. The sensitivity can be further improved by increasing the collection time. The precision, expressed as RSD, was 7.0% (n = 6) for Te. The accuracy of the method was verified using a certified reference material (GBW 07302 Stream Sediment) by aqueous standard calibration curves. The measured Te contents of the reference material was in agreement with the information value. The method was successfully applied to the determination of tellurium in coal fly ash and garlic.

  6. Genuineness assessment of mandarin essential oils employing gas chromatography-combustion-isotope ratio MS (GC-C-IRMS).

    Science.gov (United States)

    Schipilliti, Luisa; Tranchida, Peter Quinto; Sciarrone, Danilo; Russo, Marina; Dugo, Paola; Dugo, Giovanni; Mondello, Luigi

    2010-03-01

    Cold-pressed mandarin essential oils are products of great economic importance in many parts of the world and are used in perfumery, as well as in food products. Reconstituted mandarin oils are easy to find on the market; useful information on essential oil authenticity, quality, extraction technique, geographic origin and biogenesis can be attained through high-resolution GC of the volatile fraction, or enantioselective GC, using different chiral stationary phases. Stable isotope ratio analysis has gained considerable interest for the unveiling of citrus oil adulteration, detecting small differences in the isotopic carbon composition and providing plenty of information concerning the discrimination among products of different geographical origin and the adulteration of natural essential oils with synthetic or natural compounds. In the present research, the authenticity of several mandarin essential oils was assessed through the employment of GC hyphenated to isotope ratio MS, conventional GC flame ionization detector, enantioselective GC and HPLC. Commercial mandarin oils and industrial natural (declared as such) mandarin essential oils, characterized by different harvest periods and geographic origins, were subjected to analysis. The results attained were compared with those of genuine cold-pressed Italian mandarin oils, obtained during the 2008-2009 harvest season.

  7. Phenolic Compounds in Chilean Mistletoe (Quintral, Tristerix tetrandus) Analyzed by UHPLC-Q/Orbitrap/MS/MS and Its Antioxidant Properties.

    Science.gov (United States)

    Simirgiotis, Mario J; Quispe, Cristina; Areche, Carlos; Sepúlveda, Beatriz

    2016-01-01

    Mass spectrometry has become a method of choice to characterize bioactive compounds in biological samples because of its sensitivity and selectivity. Hybrid ultra-HPLC hyphenated with Orbitrap mass analyzer is an innovative state of the art technology that allows fast and accurate metabolomic analyses. In this work the metabolites of a Chilean mistletoe endemic to the VIII region of Chile were investigated for the first time using UHPLC mass analysis (UHPLC-PDA-HESI-Orbitrap MS(n)). The anthocyanins, together with the non-pigmented phenolics were fingerprinted and correlated with the antioxidant capacities measured by the bleaching of the DPPH radical, the ferric reducing antioxidant power (FRAP), the superoxide anion scavenging activity assay (SA), and total content of phenolics, flavonoids and anthocyanins measured by spectroscopic methods. Six anthocyanins were identified, and among them, the 3-O-glycosides of delphinidin and cyanidin were the major ones. In addition, several phenolic acids (including feruloylquinic acid, feruloyl glucose, chlorogenic acid) and several flavonols (luteolin, quercetin, apigenin, isorhamnetin and glycoside derivatives) were also identified. The mistletoe leaves showed the highest antioxidant activity as measured by the DPPH radical bleaching, ferric reducing antioxidant power and superoxide anion scavenging activity tests (13.38 ± 0.47 µg/mL, 125.32 ± 5.96 µmolTE/g DW and 84.06 ± 4.59 at 100 µg/mL, respectively). PMID:26907248

  8. Phenolic Compounds in Chilean Mistletoe (Quintral, Tristerix tetrandus Analyzed by UHPLC–Q/Orbitrap/MS/MS and Its Antioxidant Properties

    Directory of Open Access Journals (Sweden)

    Mario J. Simirgiotis

    2016-02-01

    Full Text Available Mass spectrometry has become a method of choice to characterize bioactive compounds in biological samples because of its sensitivity and selectivity. Hybrid ultra-HPLC hyphenated with Orbitrap mass analyzer is an innovative state of the art technology that allows fast and accurate metabolomic analyses. In this work the metabolites of a Chilean mistletoe endemic to the VIII region of Chile were investigated for the first time using UHPLC mass analysis (UHPLC-PDA-HESI-Orbitrap MSn. The anthocyanins, together with the non-pigmented phenolics were fingerprinted and correlated with the antioxidant capacities measured by the bleaching of the DPPH radical, the ferric reducing antioxidant power (FRAP, the superoxide anion scavenging activity assay (SA, and total content of phenolics, flavonoids and anthocyanins measured by spectroscopic methods. Six anthocyanins were identified, and among them, the 3-O-glycosides of delphinidin and cyanidin were the major ones. In addition, several phenolic acids (including feruloylquinic acid, feruloyl glucose, chlorogenic acid and several flavonols (luteolin, quercetin, apigenin, isorhamnetin and glycoside derivatives were also identified. The mistletoe leaves showed the highest antioxidant activity as measured by the DPPH radical bleaching, ferric reducing antioxidant power and superoxide anion scavenging activity tests (13.38 ± 0.47 µg/mL, 125.32 ± 5.96 µmolTE/g DW and 84.06 ± 4.59 at 100 µg/mL, respectively.

  9. Guaiacol and 4-methylphenol as specific markers of torrefied malts. Fate of volatile phenols in special beers through aging.

    Science.gov (United States)

    Scholtes, Caroline; Nizet, Sabrina; Collin, Sonia

    2014-10-01

    Phenol-specific extracts of 12 Belgian special beers were analyzed by gas chromatography hyphenated to olfactometry (AEDA procedure) and mass spectrometry (single ion monitoring mode). As guaiacol and 4-methylphenol were revealed to be more concentrated in brown beers (>3.5 and >1.1 μg/L, respectively), they are proposed as specific markers of the utilization of dark malts. Analysis of five differently colored malts (5, 50, 500, 900, and 1500 °EBC) allowed confirmation of high levels of guaiacol (>180 μg/L; values given in wort, for 100% specialty malt) and 4-methylphenol (>7 μg/L) for chocolate and black malts only (versus respectively beer aging highlighted major differences between phenols. Guaiacol and 4-methylphenol appeared even more concentrated in dark beers after 14 months of aging, reaching levels not far from their sensory thresholds. 4-Vinylphenols and 4-ethylphenols, on the contrary, proved to be gradually degraded in POF(+)-yeast-derived beers. Vanillin exhibited an interesting pattern: in beers initially containing Beers initially showing an above-threshold level of vanillin displayed a decrease during aging. PMID:25174984

  10. In-time and in-space tandem mass spectrometry to determine the metabolic profiling of flavonoids in a typical sweet cherry (Prunus avium L.) cultivar from Southern Italy.

    Science.gov (United States)

    Crupi, Pasquale; Genghi, Rosalinda; Antonacci, Donato

    2014-10-01

    This paper presents a comprehensive analytical methodology, based on 'in-time' and 'in-space' tandem mass spectrometry (MS) techniques, to identify and quantify flavonoid compounds in a typical Italian sweet cherry cultivar (cv. Ferrovia). Five anthocyanins, four flavan-3-ols and nine flavonols were determined by means of hyphenated high-performance liquid chromatography - multi-stage MS (HPLC-MS(n)) analyses (MS(n) up to MS(4)), among which quercetin-3-O-rutinoside-7-O-glucoside, kaempferol-3-O-rutinoside-7-O-glucoside, quercetin-3-O-galactosyl-rhamnoside and quercetin-3-O-coumaroylglucoside were tentatively identified in sweet cherries for the first time. Ultrafast HPLC and tandem MS (UHPLC-MS/MS) analyses through multiple reaction monitoring experiments showed that cyanidin-3-O-rutinoside and cyanidin-3-O-glucoside were the main anthocyanins of cv. Ferrovia at maturity. Moreover, consistent levels of catechin and epicatechin as well as quercetin-3-O-rutinoside and kaempferol-3-O-rutinoside were also found. Because flavonoids have been ascribed as potential health-promoting compounds, gathered findings provide new insight into the knowledge of the quali-quantitative profile of these phytochemicals into a widespread fruit such as sweet cherry. PMID:25303392

  11. Chemical characterization of fruit wine made from Oblačinska sour cherry.

    Science.gov (United States)

    Pantelić, Milica; Dabić, Dragana; Matijašević, Saša; Davidović, Sonja; Dojčinović, Biljana; Milojković-Opsenica, Dušanka; Tešić, Zivoslav; Natić, Maja

    2014-01-01

    This paper was aimed at characterizing the wine obtained from Oblačinska, a native sour cherry cultivar. To the best of our knowledge, this is the first paper with the most comprehensive information on chemical characterization of Oblačinska sour cherry wine. The chemical composition was characterized by hyphenated chromatographic methods and traditional analytical techniques. A total of 24 compounds were quantified using the available standards and another 22 phenolic compounds were identified based on the accurate mass spectrographic search. Values of total phenolics content, total anthocyanin content, and radical scavenging activity for cherry wine sample were 1.938 mg gallic acid eqv L(-1), 0.113 mg cyanidin-3-glucoside L(-1), and 34.56%, respectively. In general, cherry wine polyphenolics in terms of nonanthocyanins and anthocyanins were shown to be distinctive when compared to grape wines. Naringenin and apigenin were characteristic only for cherry wine, and seven anthocyanins were distinctive for cherry wine. PMID:25101316

  12. Use of time-of-flight mass spectrometry for large screening of organic pollutants in surface waters and soils from a rice production area in Colombia.

    Science.gov (United States)

    Hernández, F; Portolés, T; Ibáñez, M; Bustos-López, M C; Díaz, R; Botero-Coy, A M; Fuentes, C L; Peñuela, G

    2012-11-15

    The irrigate district of Usosaldaña, an important agricultural area in Colombia mainly devoted to rice crop production, is subjected to an intensive use of pesticides. Monitoring these compounds is necessary to know the impact of phytosanitary products in the different environmental compartments. In this work, surface water and soil samples from different sites of this area have been analyzed by applying an analytical methodology for large screening based on the use of time-of-flight mass spectrometry (TOF MS) hyphenated to liquid chromatography (LC) and gas chromatography (GC). Several pesticides were detected and unequivocally identified, such as the herbicides atrazine, diuron or clomazone. Some of their main metabolites and/or transformation products (TPs) like deethylatrazine (DEA), deisopropylatrazine (DIA) and 3,4-dichloroaniline were also identified in the samples. Among fungicides, carbendazim, azoxystrobin, propiconazole and epoxiconazole were the most frequently detected. Insecticides such as thiacloprid, or p,p'-DDT metabolites (p,p'-DDD and p,p'-DDE) were also found. Thanks to the accurate-mass full-spectrum acquisition in TOF MS it was feasible to widen the number of compounds to be investigated to other families of contaminants. This allowed the detection of emerging contaminants, such as the antioxidant 3,5-di-tertbutyl-4-hydroxy-toluene (BHT), its metabolite 3,5-di-tert-butyl-4-hydroxy-benzaldehyde (BHT-CHO), or the solar filter benzophenone, among others.

  13. PY-GC-MS applied to the identification of synthetic resins in Brazilian painting

    Energy Technology Data Exchange (ETDEWEB)

    Redigolo, Marcelo M.; Amaral, Priscila O.; Leao, Claudio; Crepaldi, Caike; Munita, Casimiro S.; Bustillos, Oscar V., E-mail: marcelo.redigolo@usp.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Russo, Tatiana; Mendonca, Valeria de [Pinacoteca do Estado de Sao Paulo, SP (Brazil)

    2015-07-01

    Works of art are appreciated for their material and immaterial value. Restoring objects of art is a delicate procedure, mostly due to the irreversibility of the interventions. Hence, it is recommended to study the chemical composition of the object to avoid errors. The premise for restoring or conserving these objects is their physical preservation, i.e., it is advisable to avoid sampling and, when necessary, samples must be minute. The analytical techniques that fulfill these requirements are limited. Mass spectrometry (MS) is a versatile technique due to its hyphenation possibilities. Recently, it has being employed in the identification of natural and synthetic resins in works of art. Electron ionization (EI) is a powerful method of molecular fragmentation employed in the detection of volatile organic compounds by mass spectrometry. In this work, two micrograms (μg) of sample from a Brazilian contemporary painting were analyzed by pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) technique. A microfurnace-type pyrolyzer was coupled to a gas chromatograph, using a non-polar capillary column. The electron ionization was achieved applying 70 eV electron energy. This technique is suitable for the analysis of material from objects of art, being specific, accurate and requiring minimal sampling. The synthetic resin diallyl phthalate (DAP) was identified by the Py-GC/MS technique. (author)

  14. EDITORIAL: Presentation of Manuscripts

    Science.gov (United States)

    Hudson, R. P.

    1984-01-01

    We wish to draw the attention of authors to two points concerning the presentation of manuscripts. First, some changes have been made recently in our Instructions to Authors. We have reduced from two to one the number of duplicate copies of the manuscript required, asked for corrected proofs to be returned to the Editor rather than directly to the publishers, clarified that a single set of illustration-photographs will suffice, removed a specific suggestion for a style manual that we had offered for general guidance only, and added an instruction on conventions in spelling and hyphenation. Secondly, authors are required, of course, to present a thorough analysis of their experimental data and to include an estimate of their uncertainty. For this purpose, however, we strongly encourage the authors to follow the recommendations put forward by an international working group [1] to the Comité International des Poids et Mesures (CIPM) and endorsed by that body in its Recommandation 1 (CI-1981). This recommendation has been published by the CIPM [2] and was also summarized recently in this journal [3]. [1] 1981 Metrologia 17 69-74, in particular, see pp 73-74 [2] 1981 ProcA~¨s-Verbaux CIPM 10th Session 49, A1 A12. An English language version is available on application to the Director of the Bureau International des Poids et Mesures. [3] 1982 Metrologia 18 41-44, in particular, see p 44.

  15. Selenium Metabolism in Cancer Cells: The Combined Application of XAS and XFM Techniques to the Problem of Selenium Speciation in Biological Systems

    Directory of Open Access Journals (Sweden)

    Hugh H. Harris

    2013-05-01

    Full Text Available Determining the speciation of selenium in vivo is crucial to understanding the biological activity of this essential element, which is a popular dietary supplement due to its anti-cancer properties. Hyphenated techniques that combine separation and detection methods are traditionally and effectively used in selenium speciation analysis, but require extensive sample preparation that may affect speciation. Synchrotron-based X-ray absorption and fluorescence techniques offer an alternative approach to selenium speciation analysis that requires minimal sample preparation. We present a brief summary of some key HPLC-ICP-MS and ESI-MS/MS studies of the speciation of selenium in cells and rat tissues. We review the results of a top-down approach to selenium speciation in human lung cancer cells that aims to link the speciation and distribution of selenium to its biological activity using a combination of X-ray absorption spectroscopy (XAS and X-ray fluorescence microscopy (XFM. The results of this approach highlight the distinct fates of selenomethionine, methylselenocysteine and selenite in terms of their speciation and distribution within cells: organic selenium metabolites were widely distributed throughout the cells, whereas inorganic selenium metabolites were compartmentalized and associated with copper. New data from the XFM mapping of electrophoretically-separated cell lysates show the distribution of selenium in the proteins of selenomethionine-treated cells. Future applications of this top-down approach are discussed.

  16. An interdisciplinary physical-chemical approach for characterization of arsenic in a calciner residue dump in Cornwall (UK)

    Energy Technology Data Exchange (ETDEWEB)

    Teun van Elteren, Johannes [National Institute of Chemistry (Kiribati), Hajdrihova 19, SI-1001, Ljubljana (Slovenia)]. E-mail: elteren@ki.si; Slejkovec, Zdenka [Jozef Stefan Institute, Jamova 39 (IJS), SI-1000 Ljubljana (Slovenia); Arcon, Iztok [Jozef Stefan Institute, Jamova 39 (IJS), SI-1000 Ljubljana (Slovenia); Nova Gorica Polytechnic (PNG), Vipavska 13, SI-5000 Nova Gorica (Slovenia); Glass, Hylke-Jan [University of Exeter in Cornwall (UEC), Tremough Campus, TR10 9EZ Penryn, Cornwall (United Kingdom)

    2006-02-15

    During the later stages of hard-rock mining in Cornwall, UK, widespread processing and refining of arsenic in purpose-built calciners resulted in severe, localized contamination of soils with arsenic. Several physical-chemical techniques were applied to characterize arsenic in a calciner residue dump: X-ray powder diffraction (XRD), sequential extraction combined with hyphenated speciation methods, and X-ray absorption spectroscopic (XAS) methods such as XANES (X-ray absorption near-edge structure) and EXAFS (extended X-ray absorption fine structure). Arsenic was predominantly present in pentavalent form, bound to amorphous or poorly-crystalline hydrous oxides of Fe (probably {alpha}-hematite). A small amount of a non-classified crystalline iron arsenate phase was found, viz. Fe{sub 2}(As(AsO{sub 4}){sub 3}). There was also evidence for the presence of some arsenate bound to quartz ({alpha}-SiO{sub 2}). The overall results make us believe that the normally assumed relative safety, from a mobility point of view, is questionable since only a small fraction of arsenic is found in a crystalline iron arsenate form. - Arsenic in calciner residue dumps is present as arsenate in crystalline (Fe{sub 2}(As(AsO{sub 4}){sub 3})) and amorphous or poorly-crystalline (bound to hematite and quartz) structures.

  17. Gas Chromatography Coupled to Atmospheric Pressure Chemical Ionization FT-ICR Mass Spectrometry for Improvement of Data Reliability.

    Science.gov (United States)

    Schwemer, Theo; Rüger, Christopher P; Sklorz, Martin; Zimmermann, Ralf

    2015-12-15

    Atmospheric pressure chemical ionization (APCI) offers the advantage of molecular ion information with low fragmentation. Hyphenating APCI to gas chromatography (GC) and ultrahigh resolution mass spectrometry (FT-ICR MS) enables an improved characterization of complex mixtures. Data amounts acquired by this system are very huge, and existing peak picking algorithms are usually extremely time-consuming, if both gas chromatographic and ultrahigh resolution mass spectrometric data are concerned. Therefore, automatic routines are developed that are capable of handling these data sets and further allow the identification and removal of known ionization artifacts (e.g., water- and oxygen-adducts, demethylation, dehydrogenation, and decarboxylation). Furthermore, the data quality is enhanced by the prediction of an estimated retention index, which is calculated simply from exact mass data combined with a double bond equivalent correction. This retention index is used to identify mismatched elemental compositions. The approach was successfully tested for analysis of semivolatile components in heavy fuel oil and diesel fuel as well as primary combustion particles emitted by a ship diesel research engine. As a result, 10-28% of the detected compounds, mainly low abundant species, classically assigned by using only the mass spectrometric information, were identified as not valid and removed. Although GC separation is limited by the slow acquisition rate of the FT-ICR MS (information.

  18. Capillary electrokinetic chromatography of insulin and related synthetic analogues.

    Science.gov (United States)

    Ortner, K; Buchberger, W; Himmelsbach, M

    2009-04-01

    With the implementation of recombinant DNA technology in the pharmaceutical industry, some synthetic insulins have been developed in order to improve the therapy of diabetes. These analogues differ only slightly in the amino acid sequence, therefore displaying a great challenge for analytical chemistry. Within the work presented in this paper, capillary zone electrophoresis (CZE), micellar electrokinetic chromatography (MEKC) with sodium dodecylsulphate (SDS) as micelle-forming agent, and microemulsion electrokinetic chromatography (MEEKC) with microemulsions consisting of SDS, n-octane and 1-butanol were investigated for the separation of human insulin and five synthetic analogues. Best results were achieved with a solvent-modified MEKC system consisting of 100mM sodium dodecyl sulphate and 15% acetonitrile in 10mM borate buffer (pH 9.2). A similar system based on perfluorooctanoic acid as micelle-forming agent in ammonium acetate (pH 9.2) was successfully employed for the hyphenation with a quadrupole/time-of-flight mass spectrometer via a sheath-flow interface. In this case, detection limits at 10mg/L could be achieved. PMID:19027906

  19. Evidence of different stoichiometries for the limiting carbonate complexes of lanthanides(3)

    International Nuclear Information System (INIS)

    Two stoichiometries have been proposed by different laboratories to interpret measurements on the limiting carbonate complexes of An3+ and Ln3+ cations. The study of the solubility of double carbonates (AlkLn(CO3)2,xH2O) in concentrated carbonate solutions at room temperature and high ionic strengths has shown that on the one hand the lightest lanthanides (La and Nd) form Ln(CO3)45- whereas the heaviest (Eu and Dy) form Ln(CO3)33- in the studied chemical conditions, and on the other hand, that the kinetics of precipitation of double carbonates depends on the alkali metal and the lanthanide ions. The existence of two stoichiometries for the limiting carbonate complexes was confirmed by capillary electrophoresis hyphenated to an inductively coupled plasma mass spectrometer (CE-ICP-MS), used to extend the study to the whole series of lanthanides (except Ce, Pm and Yb). Two behaviours have been put forward comparing the electrophoretic mobilities: La to Tb form Ln(CO3)45- while Dy to Lu form Ln(CO3)33-. Measurements by time resolved laser fluorescence spectroscopy (TRLFS) on Eu(III) indicate small variations of the geometry of Eu(CO3)33- complex, specially with Cs+. Although analogies are currently used among the 4f-block trivalent elements, different aqueous speciations are evidenced in concentrated carbonate solutions across the lanthanide series. (author)

  20. Sulfur analysis by inductively coupled plasma-mass spectrometry: A review

    International Nuclear Information System (INIS)

    In recent years the number of applications of sulfur (S) analysis using inductively coupled plasma mass spectrometry (ICP-MS) as detector has increased significantly. In this article we describe in some depth the application of ICP-MS for S analysis with emphasis placed on the sulfur-specific detection by hyphenated techniques such as LC, GC, CE and LA coupled on-line to ICP-MS. The different approaches available for sulfur isotope ratio measurements by ICP-MS are also detailed. Particular attention has been paid to the quantification of peptides/proteins and the analysis of metallopeptides/metalloproteins via sulfur by LC–ICP-MS. Likewise, the speciation analysis of metal-based pharmaceuticals and metallodrugs and non-metal selective detection of pharmaceuticals via S are highlighted. Labeling procedures for metabolic applications are also included. Finally, the measurement of natural variations in S isotope composition with multicollector ICP-MS instruments is also covered in this review. - Highlights: • Emphasis placed on the sulfur-specific detection by chromatographic techniques coupled on-line to ICP-MS. • Different instrumental approaches available for sulfur measurements by ICP-MS. • Quantification of proteins and the analysis of metalloproteins via sulfur by LC-ICP-MS. • Labelling procedures for metabolic applications are also included. • The measurement of natural variations in S isotope composition with multicollector ICP-MS

  1. Elemental speciation of neptunium in ultra trace amount ranges; Elementspeziation von Neptunium im Ultraspurenbereich

    Energy Technology Data Exchange (ETDEWEB)

    Stoebener, Nils

    2013-06-25

    In the presented work, the detection of the isotope Np-237 with resonance ionization mass spectrometry (RIMS) was developed and optimized. In RIMS, sample atoms are excited and ionized with laser radiation in several, resonant steps and are subsequently detected by a mass spectrometer. Energy levels suitable for the excitation and ionization of Np-237 were identified using resonance ionization spectroscopy (RIS). With RIS, more than 300 previously unknown electronic states and autoionizing resonances of Np-237 were identified. Using in-source-RIMS, a limit of detection of 9E+5 atoms was demonstrated for the isotope. The mobility of Np in the environment strongly depends on its elemental speciation. Therefore, safety assessments of proposed nuclear waste repositories require analytical methods for the detection of Np species. CE (capillary electrophoresis) was hyphenated to ICP-MS (inductively coupled plasma mass spectrometry) to examine the distribution of the Np redox species Np(IV) and Np(V), which was possible at Np concentrations as low as 1E-9 mol/L. The method was used to study the interaction of the element with Opalinus Clay at varying conditions. CE-ICP-MS revealed, that under the presence of Fe(II), Np(V) is reduced to Np(IV), which is sorbed onto the clay. This leads to a higher overall Np sorption.

  2. Chemometrics: A new scenario in herbal drug standardization

    Directory of Open Access Journals (Sweden)

    Ankit Bansal

    2014-08-01

    Full Text Available Chromatography and spectroscopy techniques are the most commonly used methods in standardization of herbal medicines but the herbal system is not easy to analyze because of their complexity of chemical composition. Many cutting-edge analytical technologies have been introduced to evaluate the quality of medicinal plants and significant amount of measurement data has been produced. Chemometric techniques provide a good opportunity for mining more useful chemical information from the original data. Then, the application of chemometrics in the field of medicinal plants is spontaneous and necessary. Comprehensive methods and hyphenated techniques associated with chemometrics used for extracting useful information and supplying various methods of data processing are now more and more widely used in medicinal plants, among which chemometrics resolution methods and principal component analysis (PCA are most commonly used techniques. This review focuses on the recent various important analytical techniques, important chemometrics tools and interpretation of results by PCA, and applications of chemometrics in quality evaluation of medicinal plants in the authenticity, efficacy and consistency.

  3. Atmospheric pressure gas chromatography coupled to quadrupole-time of flight mass spectrometry as a tool for identification of volatile migrants from autoadhesive labels used for direct food contact.

    Science.gov (United States)

    Canellas, Elena; Vera, Paula; Nerín, Cristina

    2014-11-01

    Pressure-sensitive adhesives (PSA) are used to manufacture labels that are applied directly on the food. These adhesives could contain not only intentionally added compounds (IAS) to the adhesive formula but also non-intentionally added substances (NIAS), due to the impurities from the raw materials used, decomposition of the initial components or from chemical interactions between them. These compounds could migrate to the food and contaminate it. In this study, gas chromatography coupled with mass spectrometry (GC-MS/Q) and atmospheric pressure gas chromatography coupled to a quadrupole hyphenated to a time of flight mass spectrometer (APGC-MS/Q-TOF) have been used for identification of unknown compounds and NIAS coming from a PSA. Seven compounds were identified by GC-MS/Q, and other eight compounds remained initially unknown. The structure of these eight new compounds was elucidated by working with the spectra obtained by APGC-MS/Q-TOF. Finally, two different migration studies were carried out. The first one with Tenax as solid food simulant in contact with the paper label containing the adhesive and the second one with isooctane filled in a natural pork intestine where the label containing the adhesive was applied on the external side. The results are shown and discussed.

  4. On-line two-dimensional capillary electrophoresis with mass spectrometric detection using a fully electric isolated mechanical valve.

    Science.gov (United States)

    Kohl, Felix J; Montealegre, Cristina; Neusüß, Christian

    2016-04-01

    CE is becoming more and more important in many fields of bioanalytical chemistry. Besides optical detection, hyphenation to ESI-MS detection is increasingly applied for sensitive identification purposes. Unfortunately, many CE techniques and methods established in research and industry are not compatible to ESI-MS since essential components of the background electrolyte interfere in ES ionization. In order to identify unknown peaks in established CE methods, here, a heart-cut 2D-CE separation system is introduced using a fully isolated mechanical valve with an internal loop of only 20 nL. In this system, the sample is separated using potentially any non-ESI compatible method in the first separation dimension. Subsequently, the portion of interest is cut by the internal sample loop of the valve and reintroduced to the second dimension where the interfering compounds are removed, followed by ESI-MS detection. When comparing the separation efficiency of the system with the valve to a system using a continuous capillary only a slight increase in peak width is observed. Ultraviolet/visible detection is integrated in the first dimension for switching time determination, enabling reproducible cutting of peaks of interest. The feasibility of the system is successfully demonstrated by a 2D analysis of a BSA tryptic digest sample using a nonvolatile (phosphate based) background electrolyte in the first dimension.

  5. Advancing towards universal screening for organic pollutants in waters.

    Science.gov (United States)

    Hernández, Félix; Ibáñez, María; Portolés, Tania; Cervera, María I; Sancho, Juan V; López, Francisco J

    2015-01-23

    Environmental analytical chemists face the challenge of investigating thousands of potential organic pollutants that may be present in the aquatic environment. High resolution mass spectrometry (HRMS) hyphenated to chromatography offers the possibility of detecting a large number of contaminants without pre-selection of analytes due to its accurate-mass full-spectrum acquisition at good sensitivity. Interestingly, large screening can be made even without reference standards, as the valuable information provided by HRMS allows the tentative identification of the compound detected. In this work, hybrid quadrupole time-of-flight (QTOF) MS was combined with both liquid and gas chromatography (using a single instrument) for screening of around 2000 compounds in waters. This was feasible thanks to the use of atmospheric pressure chemical ionization source in GC. The screening was qualitatively validated for around 300 compounds at three levels (0.02, 0.1, 0.5μg/L), and screening detection limits were established. Surface, ground water and effluent wastewater samples were analyzed, detecting and identifying a notable number of pesticides and transformation products, pharmaceuticals, personal care products, and illicit drugs, among others. This is one of the most universal approaches in terms of comprehensive measurement for broad screening of organic contaminants within a large range of polarity and volatility in waters. PMID:25204505

  6. Field cryofocussing hydride generation applied to the simultaneous multi-elemental determination of alkyl-metal(loid) species in natural waters using ICP-MS detection.

    Science.gov (United States)

    Tseng, C M; Amouroux, D; Brindle, I D; Donard, O F

    2000-12-01

    Two hydride generation manifold systems, utilizing flow injection and cryotrapping techniques for alkyl-metal(loid) speciation analysis in natural waters, are described in this paper. They provide shipboard capacity for simultaneous derivatization of analytes with NaBH4 and cryotrapping of the generated products in a field packed column at -196 degrees C. The first system is a large-volume hydride generator, using a reagent-injection flow technique as a flow batch type, that has been fully optimized and applied to the simultaneous detection of alkylated species in estuarine waters. The technique permits the analysis of a large volume sample (0.5-11) at a sampling rate of 3 h-1. The second is an online continuous flow hydride generator. A sampling rate of 3-12 h-1 can be achieved with samples of 0.1-0.51. In addition, shipboard operation eliminates major problems related to sample pretreatment, transport and storage. Ultra-trace multi-element determination is finally performed in the laboratory by cryogenic GC hyphenated with ICP-MS. Routine detection limits of 0.5-10 pg (as metal) for 0.51 water samples were achieved for the selected alkyl-metal(loid) species of arsenic, germanium, mercury and tin. Concentrations of various species, obtained from water samples taken from the Rhine estuary, are also presented. These species include alkylated arsenic compounds, other than methyl derivatives, that have been tentatively identified and are reported here for the first time.

  7. Chemometric analysis of comprehensive LC×LC-MS data: Resolution of triacylglycerol structural isomers in corn oil.

    Science.gov (United States)

    Navarro-Reig, Meritxell; Jaumot, Joaquim; van Beek, Teris A; Vivó-Truyols, Gabriel; Tauler, Romà

    2016-11-01

    Comprehensive hyphenated two-dimensional liquid chromatography mass spectrometry (LC×LC-MS) is a very powerful analytical tool achieving high throughput resolution of highly complex natural samples. However, even using this approach there is still the possibility of not resolving some of the analytes of interest. For instance, triacylglycerols (TAGs) structural isomers in oil samples are extremely difficult to separate chromatographically due to their very similar structure and chemical properties. Traditional approaches based on current vendor chromatographic software cannot distinguish these isomers from their different mass spectral features. In this work, a chemometric approach is proposed to solve this problem. First, the experimental LC×LC-MS data structure is discussed, and results achieved by different methods based on the fulfilment of the trilinear model are compared. Then, the step-by-step resolution and identification of strongly coeluted compounds from different examples of triacylglycerols (TAGs) structural isomers in corn oil samples are described. As a conclusion, the separation power of two-dimensional chromatography can be significantly improved when it is combined with the multivariate curve resolution method. PMID:27591659

  8. Advancements in waste water characterization through NMR spectroscopy: review.

    Science.gov (United States)

    Alves Filho, Elenilson G; Alexandre e Silva, Lorena M; Ferreira, Antonio G

    2015-09-01

    There are numerous organic pollutants that lead to several types of ecosystem damage and threaten human health. Wastewater treatment plants are responsible for the removal of natural and anthropogenic pollutants from the sewage, and because of this function, they play an important role in the protection of human health and the environment. Nuclear magnetic resonance (NMR) has proven to be a valuable analytical tool as a result of its versatility in characterizing both overall chemical composition as well as individual species in a wide range of mixtures. In addition, NMR can provide physical information (rigidity, dynamics, etc.) as well as permit in depth quantification. Hyphenation with other techniques such as liquid chromatography, solid phase extraction and mass spectrometry creates unprecedented capabilities for the identification of novel and unknown chemical species. Thus, NMR is widely used in the study of different components of wastewater, such as complex organic matter (fulvic and humic acids), sludge and wastewater. This review article summarizes the NMR spectroscopy methods applied in studies of organic pollutants from wastewater to provide an exhaustive review of the literature as well as a guide for readers interested in this topic. PMID:25280056

  9. Optimized synthesis of L-sorbose by C(5)-dehydrogenation of D-sorbitol with Gluconobacter oxydans.

    Science.gov (United States)

    De Wulf, P; Soetaert, W; Vandamme, E J

    2000-08-01

    The optimization of L-sorbose synthesis by regiospecific dehydrogenation of D-sorbitol using Gluconobacter oxydans is reported. The current L-sorbose production processes that are based on G. oxydans and other bacterial strains are suboptimal as to yield and rate of L-sorbose synthesis. One reason for these problems is the toxicity that is induced by the substrate D-sorbitol when used in concentrations of >10% (w/v). This phenomenon significantly limits the potentials of L-sorbose production from an industrial point of view. The goal of this study was to develop a fast production process that yields L-sorbose in stoichiometric amounts starting from D-sorbitol concentrations that exceed 10% (w/v). A gradual improvement of the inoculum build-up procedure, culture medium composition, and process parameters ultimately led to a theoretically maximal L-sorbose productivity (200 g L(-1) of L-sorbose from 200 g L(-1) of D-sorbitol in 28 h of fermentation) using a Gluconobacter oxydans mutant strain that was selected under conditions of substrate inhibition. Because the D-sorbitol/L&HYPHEN;sorbose bioconversion is used to mass-produce vitamin C, the procedure reported here will contribute to a more efficient and more economic synthesis of vitamin C.

  10. Tracing gadolinium-based contrast agents from surface water to drinking water by means of speciation analysis.

    Science.gov (United States)

    Birka, Marvin; Wehe, Christoph A; Hachmöller, Oliver; Sperling, Michael; Karst, Uwe

    2016-04-01

    In recent decades, a significant amount of anthropogenic gadolinium has been released into the environment as a result of the broad application of contrast agents for magnetic resonance imaging (MRI). Since this anthropogenic gadolinium anomaly has also been detected in drinking water, it has become necessary to investigate the possible effect of drinking water purification on these highly polar microcontaminats. Therefore, a novel highly sensitive method for speciation analysis of gadolinium is presented. For that purpose, the hyphenation of hydrophilic interaction liquid chromatography (HILIC) and inductively coupled plasma-mass spectrometry (ICP-MS) was employed. In order to enhance the detection power, sample introduction was carried out by ultrasonic nebulization. In combination with a novel HILIC method using a diol-based stationary phase, it was possible to achieve superior limits of detection for frequently applied gadolinium-based contrast agents below 20pmol/L. With this method, the contrast agents Gd-DTPA, Gd-DOTA and Gd-BT-DO3A were determined in concentrations up to 159pmol/L in samples from several waterworks in a densely populated region of Germany alongside the river Ruhr as well as from a waterworks near a catchment lake. Thereby, the direct impact of anthropogenic gadolinium species being present in the surface water on the amount of anthropogenic gadolinium in drinking water was shown. There was no evidence for the degradation of contrast agents, the release of Gd(3+) or the presence of further Gd species.

  11. Metallomics:An integrated biometal science

    Institute of Scientific and Technical Information of China (English)

    2009-01-01

    Metallomics is an emerging scientific area integrating the research fields related to the understanding of the molecular mechanisms of metal-associated life processes and the entirety of metal and metalloid species within a cell or tissue type. In metallomics,metalloproteins,metalloenzymes and other metal-containing biomolecules in a biological system are referred to as metallomes,similar to genomes and proteomes in genomics and proteomics,respectively. This review discusses the concept of metallomics with a focus on analytical techniques and methods,particularly the so-called hyphenated techniques which combine a high-resolution separation technique (gel electrophoresis/laser ablation,chromatography or capillary electrophoresis) with a highly sensitive detection method such as elemental (inductively coupled plasma,ICP) or molecular (electron spray ionization (ESI) or matrix-assisted laser desorption/ionization (MALDI)) mass spectrometry,or nuclear X-ray fluorescence/absorption spectrometry. The applications of these advanced analytical methods in the identification of metallo-/phospho-/seleno-proteins,probing of relationships between structure and function of metal-loproteins,and study of clinically used metallodrugs will be selectively outlined,along with their advantages and limitations.

  12. A single sorbent for tetracycline enrichment and subsequent solid-matrix time-resolved luminescence

    Energy Technology Data Exchange (ETDEWEB)

    Liu Linshu [Eastern Regional Research Center, Agriculture Research Service, US Department of Agriculture, 600 East Mermaid Lane, Wyndmoor, PA 19038 (United States)]. E-mail: lsliu@errc.ars.usda.gov; Chen Guoying [Eastern Regional Research Center, Agriculture Research Service, US Department of Agriculture, 600 East Mermaid Lane, Wyndmoor, PA 19038 (United States); Fishman, Marshall L. [Eastern Regional Research Center, Agriculture Research Service, US Department of Agriculture, 600 East Mermaid Lane, Wyndmoor, PA 19038 (United States)

    2005-01-10

    The aim of this study was to search for a sorbent that could act as an extraction phase and as a support for solid-matrix time-resolved luminescence (SMTRL). Four potential sorbents were investigated for this purpose using tetracycline (TC) as a model analyte. Sorbents prepared from C18 silica gel or calcium cross-linked pectin gel were able to extract TC from dilute solutions. Europium(III)-TC complex adsorbed on the surface of C18 generated the most intense TRL signal when measured at {lambda}{sub ex} = 388 nm and {lambda}{sub em} = 615 nm. This method achieved a 1 ng/ml limit of detection (LOD) with a 100 {mu}l sample solution in a repeated spotting mode. Hyphenation of sorbent extraction and SMTRL was demonstrated using C18. This method is suitable for screening of TC in foods or aqueous solutions and can be extended to other luminescent lanthanide-chelating analytes in physiological or environmental samples.

  13. Tracing gadolinium-based contrast agents from surface water to drinking water by means of speciation analysis.

    Science.gov (United States)

    Birka, Marvin; Wehe, Christoph A; Hachmöller, Oliver; Sperling, Michael; Karst, Uwe

    2016-04-01

    In recent decades, a significant amount of anthropogenic gadolinium has been released into the environment as a result of the broad application of contrast agents for magnetic resonance imaging (MRI). Since this anthropogenic gadolinium anomaly has also been detected in drinking water, it has become necessary to investigate the possible effect of drinking water purification on these highly polar microcontaminats. Therefore, a novel highly sensitive method for speciation analysis of gadolinium is presented. For that purpose, the hyphenation of hydrophilic interaction liquid chromatography (HILIC) and inductively coupled plasma-mass spectrometry (ICP-MS) was employed. In order to enhance the detection power, sample introduction was carried out by ultrasonic nebulization. In combination with a novel HILIC method using a diol-based stationary phase, it was possible to achieve superior limits of detection for frequently applied gadolinium-based contrast agents below 20pmol/L. With this method, the contrast agents Gd-DTPA, Gd-DOTA and Gd-BT-DO3A were determined in concentrations up to 159pmol/L in samples from several waterworks in a densely populated region of Germany alongside the river Ruhr as well as from a waterworks near a catchment lake. Thereby, the direct impact of anthropogenic gadolinium species being present in the surface water on the amount of anthropogenic gadolinium in drinking water was shown. There was no evidence for the degradation of contrast agents, the release of Gd(3+) or the presence of further Gd species. PMID:26931429

  14. A neuron-in-capillary platform for facile collection and mass spectrometric characterization of a secreted neuropeptide

    Science.gov (United States)

    Lee, Chang Young; Fan, Yi; Rubakhin, Stanislav S.; Yoon, Sook; Sweedler, Jonathan V.

    2016-06-01

    The integration of microfluidic devices—which efficiently handle small liquid volumes—with separations/mass spectrometry (MS) is an effective approach for profiling the neurochemistry occurring in selected neurons. Interfacing the microfluidic cell culture to the mass spectrometer is challenging because of geometric and scaling issues. Here we demonstrate the hyphenation of a neuron-in-capillary platform to a solid phase extraction device and off-line MS. A primary neuronal culture of Aplysia californica neurons was established directly inside a cylindrical polyimide capillary. The approach also uses a particle-embedded monolith to condition neuropeptide releasates collected from several Aplysia neurons cultured in the capillary, with the subsequent characterization of released peptides via MS. This system presents a number of advances compared to more traditional microfluidic devices fabricated with polydimethylsiloxane. These include low cost, easy access to cell culture, rigidity, ease of transport, and minimal fluid handling. The cylindrical geometry of the platform allows convenient interface with a wide range of analytical tools that utilize capillary columns.

  15. A special reactor design for investigations of mixing time effects in a scaled-down industrial L-lysine fed-batch fermentation process

    Science.gov (United States)

    Schilling; Pfefferle; Bachmann; Leuchtenberger; Deckwer

    1999-09-01

    A specially designed model reactor based on a 42-L laboratory fermentor was equipped with six stirrers (Rushton turbines) and five cylindrical disks. In this model reactor, the mixing time, Theta(90), turned out to be 13 times longer compared with the 42-L standard laboratory fermentor fitted with two Rushton turbines and four wall-fixed longitudinal baffles. To prove the suitability of the model reactor for scaledown studies of mixing-time-dependent processes, parallel exponential fed-batch cultivations were carried out with the leucine-auxotrophic strain, Corynebacterium glutamicum DSM 5715, serving as a microbial test system. L&HYPHEN;Leucine, the process-limiting substrate, was fed onto the liquid surface of both reactors. Cultivations were conducted using the same inoculum material and equal oxygen supply. The model reactor showed reduced sugar consumption (-14%), reduced ammonium consumption (-19%), and reduced biomass formation (-7%), which resulted in a decrease in L-lysine formation (-12%). These findings were reflected in less specific enzyme activity, which was determined for citrate synthase (CS), phosphoenolpyruvate carboxylase (PEP-C), and aspartate kinase (AK). The reduced specific activity of CS correlated with lower CO(2) evolution (-36%) during cultivation. The model reactor represents a valuable tool to simulate the conditions of poor mixing and inhomogeneous substrate distribution in bioreactors of industrial scale. Copyright 1999 John Wiley & Sons, Inc.

  16. Mercury speciation by CE: an update.

    Science.gov (United States)

    Kubán, Petr; Pelcová, Pavlína; Margetínová, Jana; Kubán, Vlastimil

    2009-01-01

    This review provides an update on mercury speciation by CE. It includes a brief discussion on physicochemical properties, toxicity and transformation pathways of mercury species (i.e. methyl-, ethyl-, phenyl- and inorganic mercury) and outlines recent trends in Hg speciation by CE. CE is presented as a complementary technique to chromatographic separation techniques, especially in cases when speed, high efficiency and low sample volumes are required. The development of suitable sample preconcentration/isolation (sample stacking, ion exchange, liquid-liquid-liquid extraction, dual-cloud point extraction) to achieve low LODs for analysis of trace concentrations of mercury species in real samples is emphasized. Hyphenation of CE to element specific detectors (i.e. electrothermal atomic absorption spectrometry, atomic fluorescence spectrometry, inductively coupled plasma-optical emission spectrometry, inductively coupled plasma-mass spectrometry) is discussed as well as a potential of CE in interaction studies that may provide useful information on interaction of various Hg species with selected bio-macromolecules.

  17. Assessment of trace aluminium content in parenteral solutions by combined cloud point preconcentration-flow injection inductively coupled plasma optical emission spectrometry.

    Science.gov (United States)

    Sombra, Lorena L; Luconi, Marta O; Fernández, Liliana P; Olsina, Roberto A; Silva, María F; Martínez, Luis D

    2003-01-01

    A micelle-mediated phase separation without added chelating agents to preconcentrate trace levels of aluminium in parenteral solutions as a prior step to its determination by flow injection inductively coupled plasma optical emission spectrometry has been developed. The enrichment step is based on the cloud point extraction of aluminium with the non-ionic surfactant polyethyleneglycolmono-p-nonylphenylether (PONPE 7.5). The chemical variables affecting the sensitivity of the extractive-spectrometric procedure were studied in detail. After optimization, a preconcentration factor of 200 and a %E higher than 99.9 were achieved. The detection limit (DL) value of aluminium for the preconcentration of 50 ml of parenteral solution was 0.25 microgl(-1). The calibration graph using the preconcentration system for aluminium was linear with a correlation coefficient of 0.9997 at levels near the DLs up to at least 200 microgl(-1). The developed hyphenated assay, which thoroughly satisfies the typical requirements for pharmaceutical control processes, is appropriate to monitor the aluminium concentration in parenteral nutrition.

  18. Challenges in medical education: the Family Health Program as educational practice Desafios na formação médica: o Programa Saúde da Família como prática de ensino

    Directory of Open Access Journals (Sweden)

    Eluiza Helena Leite Arias

    2010-11-01

    Full Text Available

    A relação médico-paciente, substância essencial do ato médico, vem ao longo da evolução do exercício da medicina, sofrendo mudanças, perdendo a cada dia, características fundamentais, como a humanização, a ética e a comunicação. Aborda a questão da percepção do aluno da medicina sobre a relação médicopaciente, a importância da família nesta relação, e a experiencia do trabalho em equipe. A hipótese central e que o aluno desenvolvendo a prática de ensino no Programa Saude da Familia (PSF, modelo assistencial tendo como núcleo central a fam

  19. Anionic metabolite profiling by capillary electrophoresis-mass spectrometry using a noncovalent polymeric coating. Orange juice and wine as case studies.

    Science.gov (United States)

    Acunha, Tanize; Simó, Carolina; Ibáñez, Clara; Gallardo, Alberto; Cifuentes, Alejandro

    2016-01-01

    In several metabolomic studies, it has already been demonstrated that capillary electrophoresis hyphenated to mass spectrometry (CE-MS) can detect an important group of highly polar and ionized metabolites that are overseen by techniques such as NMR, LC-MS and GC-MS, providing complementary information. In this work, we present a strategy for anionic metabolite profiling by CE-MS using a cationic capillary coating. The polymer, abbreviated as PTH, is composed of a poly-(N,N,N',N'-tetraethyldiethylenetriamine, N-(2-hydroxypropyl) methacrylamide, TEDETAMA-co-HPMA (50:50) copolymer. A CE-MS method based on PTH-coating was optimized for the analysis of a group of 16 standard anionic metabolites. Separation was achieved within 12min, with high separation efficiency (up to 92,000 theoretical plates per meter), and good repeatability, namely, relative standard deviation values for migration times and peak areas were below 0.2 and 2.1%, respectively. The optimized method allowed the detection of 87 metabolites in orange juice and 142 metabolites in red wine, demonstrating the good possibilities of this strategy for metabolomic applications.

  20. Electrochemical methods in conjunction with capillary and microchip electrophoresis.

    Science.gov (United States)

    Mark, Jonas J P; Scholz, Rebekka; Matysik, Frank-Michael

    2012-12-01

    Electromigrative techniques such as capillary and microchip electrophoresis (CE and MCE) are inherently associated with various electrochemical phenomena. The electrolytic processes occurring in the buffer reservoirs have to be considered for a proper design of miniaturized electrophoretic systems and a suitable selection of buffer composition. In addition, the control of the electroosmotic flow plays a crucial role for the optimization of CE/MCE separations. Electroanalytical methods have significant importance in the field of detection in conjunction with CE/MCE. At present, amperometric detection and contactless conductivity detection are the predominating electrochemical detection methods for CE/MCE. This paper reviews the most recent trends in the field of electrochemical detection coupled to CE/MCE. The emphasis is on methodical developments and new applications that have been published over the past five years. A rather new way for the implementation of electrochemical methods into CE systems is the concept of electrochemically assisted injection which involves the electrochemical conversions of analytes during the injection step. This approach is particularly attractive in hyphenation to mass spectrometry (MS) as it widens the range of CE-MS applications. An overview of recent developments of electrochemically assisted injection coupled to CE is presented.

  1. Characterization of petroleum distillates by GC-AED (coupling with gas chromatography and atomic emission detection); Caracterisation des distillats petroliers par couplage chromatographie en phase gazeuse et detection par emission atomique

    Energy Technology Data Exchange (ETDEWEB)

    Baco, F.

    1997-05-21

    This thesis describes the characterization of atmospheric petroleum distillates (kerosenes and gas-oils) and vacuum distillates by hyphenated technic of Gas Chromatography and Atomic Emission Detector (GC-AED). A gas chromatographic simulated distillation, which gives the weight % of sample as a function of the petroleum cut temperature, was adapted to the GC-AED to obtain an original information about the elemental composition profile. After generalities, historic of the development of the instrument and the first petroleum applications are described. In the experimental part, analytical conditions used, different technics of characterisation of distillates and the base of samples analyzed are exposed. After a study of the GC-AED`s performances for the target elements (C, H, S, N), a quantitative method for the elemental analysis of distillates was developed and validated at three levels: total elemental analysis, simulated distillation and elemental composition as a function of the distillation profile. Finally, different ways for the applications of the GC-AED in order to characterize the distillates were explored, in particular to classify products and predict some petroleum properties (cetane number, density,...). The more interesting outlook seems to be the prediction of some properties as a function of the distillation profile. (author) 155 refs.

  2. Ultrafast 2D NMR: An Emerging Tool in Analytical Spectroscopy

    Science.gov (United States)

    Giraudeau, Patrick; Frydman, Lucio

    2014-06-01

    Two-dimensional nuclear magnetic resonance (2D NMR) spectroscopy is widely used in chemical and biochemical analyses. Multidimensional NMR is also witnessing increased use in quantitative and metabolic screening applications. Conventional 2D NMR experiments, however, are affected by inherently long acquisition durations, arising from their need to sample the frequencies involved along their indirect domains in an incremented, scan-by-scan nature. A decade ago, a so-called ultrafast (UF) approach was proposed, capable of delivering arbitrary 2D NMR spectra involving any kind of homo- or heteronuclear correlation, in a single scan. During the intervening years, the performance of this subsecond 2D NMR methodology has been greatly improved, and UF 2D NMR is rapidly becoming a powerful analytical tool experiencing an expanded scope of applications. This review summarizes the principles and main developments that have contributed to the success of this approach and focuses on applications that have been recently demonstrated in various areas of analytical chemistry—from the real-time monitoring of chemical and biochemical processes, to extensions in hyphenated techniques and in quantitative applications.

  3. Punctuation as readability and textuality factor in technical discourse

    Directory of Open Access Journals (Sweden)

    Carmen Sancho Guinda

    2002-04-01

    Full Text Available This paper studies the incidence of punctuation on the reading comprehension of technical discourse and its role as a factor of textuality. Starting out from the notions of textuality and punctuation functions formulated by different linguistic approaches, an analysis has been made to quantify the decoding skills and punctuating competence of 60 Aeronautical Engineering students, as well as to determine the nature and effects of their punctuation errors. The survey has been focused on the Full Stop, the comma and the hyphen due to their highly conflicting uses as regards the identification of immediate sentence constituents and semantic relationships. The results obtained suggest that most students have a poor knowledge of punctuation rules and little awareness of punctuation as a textual elementaffecting readability. Errors are in the main related to comma use and produced by transference, either of Spanish punctuating habits into English, or of individual prosodic patterns into writing, while meaning appears to be the prevailing punctuating criterion over sound and syntax. Punctuation proves an effective tool for the anticipation of implicit meanings and an untapped resource in the teaching of the diverse communicative and stylistic possibilities offered by technical texts.

  4. A educação cooperativa numa perspectiva marxista

    Directory of Open Access Journals (Sweden)

    Antonio Inacio Andrioli

    2009-12-01

    Full Text Available

    Granulomatosis peritoneal por Ascaris lumbricoides.Presentación de un caso Granulomatous peritonitis due to Ascaris lumbricoides. Case report

    Directory of Open Access Journals (Sweden)

    Carlos Aguirre Muñoz

    2008-06-01

    Full Text Available

    La ascariasis es una parasitosis ampliamente diseminada en el mundo, especialmente en los niños de los países en vías de desarrollo, ligada a condiciones de pobreza, desnutrición y mala higiene. Se acepta que es la geohelmintiasis más frecuente entre todas

  5. [E]motion in the Nineteenth Century: A Culture of Fidgets

    Directory of Open Access Journals (Sweden)

    Karen Chase

    2014-10-01

    Full Text Available I see the fidget as a neglected aspect of the sense of touch, which collects a range of suggestive imaginative movements and which opens towards a rereading of Dickens's construal of character, its relation to the self, and its social world. An affective swamping of personality repeatedly overwhelms the barriers of personality. A tic, a flick, an insult, a plea, a joke, a contortion, a wink, a tickle, a prod - such fidgets lead an active life in the novels. They often reflect the friction of inter-subjectivity, but also the abrasions between character and the universe of objects. The twittering of a Miss Flite in 'Bleak House', Bradley Headstone's physical eruptions of rage, Mr F's Aunt's proleptic warnings and Flora Finching's galloping tale-telling in 'Little Dorrit', the handiwork of Uriah Heep in 'David Copperfield', the insuppressible hyphenated speech of Jingle in 'Pickwick Papers' - these are radiant instances. My article looks to give the fidget its due and to initiate more scholarly conversation on the circle of issues that it generates: mind and body, subjects and objects, textual continuity and its disruptions.

  6. Analytical methods for the extraction and identification of secondary metabolite production in 'in vitro' plant cell cultures.

    Science.gov (United States)

    Bertoli, Alessandra; Ruffoni, Barbara; Pistelli, Laura; Pistelli, Luisa

    2010-01-01

    The production of plant secondary metabolites by in vitro culture is one of the most challenging and thrilling field of recent scientific researches. In the few last years, pharmaceutical and food industry demand in phytochemicals has increased steadily. Therefore, the establishment of in vitro plant protocols has to be monitored by phytochemical investigation of their selected extracts in order to supply standardized raw material. In this chapter, the advantages and disadvantages of some modem techniques have been described for the sampling, extraction and analysis ofthe invitro plants and derivatives. Depending on the volatile or nonvolatile substances produced by in vitro plant raw material, different kinds of laboratory facilities are needed for the extraction and quali-quantitative analysis. Recent extraction technology such as accelerated solvent extraction or microwave assisted extraction in combination with hyphenated techniques such as gas chromathography-mass spectrometry (GC-MS) and liquid chromatography-mass spectrometry (LC-MS) represent a modern approach to perform fast and reproducible analytical methods for the quality control of secondary metabolite production in 'in vitro' plant material. PMID:21520717

  7. An interdisciplinary physical-chemical approach for characterization of arsenic in a calciner residue dump in Cornwall (UK).

    Science.gov (United States)

    van Elteren, Johannes Teun; Slejkovec, Zdenka; Arcon, Iztok; Glass, Hylke-Jan

    2006-02-01

    During the later stages of hard-rock mining in Cornwall, UK, widespread processing and refining of arsenic in purpose-built calciners resulted in severe, localized contamination of soils with arsenic. Several physical-chemical techniques were applied to characterize arsenic in a calciner residue dump: X-ray powder diffraction (XRD), sequential extraction combined with hyphenated speciation methods, and X-ray absorption spectroscopic (XAS) methods such as XANES (X-ray absorption near-edge structure) and EXAFS (extended X-ray absorption fine structure). Arsenic was predominantly present in pentavalent form, bound to amorphous or poorly-crystalline hydrous oxides of Fe (probably alpha-hematite). A small amount of a non-classified crystalline iron arsenate phase was found, viz. Fe2(As(AsO4)3). There was also evidence for the presence of some arsenate bound to quartz (alpha-SiO2). The overall results make us believe that the normally assumed relative safety, from a mobility point of view, is questionable since only a small fraction of arsenic is found in a crystalline iron arsenate form.

  8. Analytical methods for the endocrine disruptor compounds determination in environmental water samples.

    Science.gov (United States)

    Locatelli, Marcello; Sciascia, Francesco; Cifelli, Roberta; Malatesta, Luciano; Bruni, Pantaleone; Croce, Fausto

    2016-02-19

    The potential risk of exposure to different xenobiotics, which can modulate the endocrine system and represent a treat for the wellness of an increasing number of people, has recently drawn the attention of international environmental and health agencies. Several agents, characterized by structural diversity, may interfer with the normal endocrine functions that regulate cell growth, homeostasis and development. Substances such as pesticides, herbicides, plasticizers, metals, etc. having endocrine activity (EDCs) are used in agriculture and industry and are also used as drugs for humans and animals. A difficulty in the analytical determination of these substances is the complexity of the matrix in which they are present. In fact, the samples most frequently analyzed consist of groundwater and surface water, including influent and effluent of wastewater treatment plants and drinking water. In this review, several sample pretreatment protocols, assays and different instrumental techniques recently used in the EDCs determination have been considered. This review concludes with a paragraph in which the most recent hyphenated-instrument techniques are treated, highlighting their sensitivity and selectivity for the analyses of environmental water samples. PMID:26805600

  9. Forensic Mass Spectrometry

    Science.gov (United States)

    Hoffmann, William D.; Jackson, Glen P.

    2015-07-01

    Developments in forensic mass spectrometry tend to follow, rather than lead, the developments in other disciplines. Examples of techniques having forensic potential born independently of forensic applications include ambient ionization, imaging mass spectrometry, isotope ratio mass spectrometry, portable mass spectrometers, and hyphenated chromatography-mass spectrometry instruments, to name a few. Forensic science has the potential to benefit enormously from developments that are funded by other means, if only the infrastructure and personnel existed to adopt, validate, and implement the new technologies into casework. Perhaps one unique area in which forensic science is at the cutting edge is in the area of chemometrics and the determination of likelihood ratios for the evaluation of the weight of evidence. Such statistical techniques have been developed most extensively for ignitable-liquid residue analyses and isotope ratio analysis. This review attempts to capture the trends, motivating forces, and likely impact of developing areas of forensic mass spectrometry, with the caveat that none of this research is likely to have any real impact in the forensic community unless: (a) The instruments developed are turned into robust black boxes with red and green lights for positives and negatives, respectively, or (b) there are PhD graduates in the workforce who can help adopt these sophisticated techniques.

  10. A two-level model for evidence evaluation in the presence of zeros.

    Science.gov (United States)

    Zadora, Grzegorz; Neocleous, Tereza; Aitken, Colin

    2010-03-01

    Likelihood ratios (LRs) provide a natural way of computing the value of evidence under competing propositions. We propose LR models for classification and comparison that extend the ideas of Aitken, Zadora, and Lucy and Aitken and Lucy to include consideration of zeros. Instead of substituting zeros by a small value, we view the presence of zeros as informative and model it using Bernoulli distributions. The proposed models are used for evaluation of forensic glass (comparison and classification problem) and paint data (comparison problem). Two hundred and sixty-four glass samples were analyzed by scanning electron microscopy, coupled with an energy dispersive X-ray spectrometer method and 36 acrylic topcoat paint samples by pyrolysis gas chromatography hyphened with mass spectrometer method. The proposed LR model gave very satisfactory results for the glass comparison problem and for most of the classification tasks for glass. Results of comparison of paints were also highly satisfactory, with only 3.0% false positive answers and 2.8% false negative answers.

  11. Medicinal plants in the treatment of women's disorders: Analytical strategies to assure quality, safety and efficacy.

    Science.gov (United States)

    Masullo, Milena; Montoro, Paola; Mari, Angela; Pizza, Cosimo; Piacente, Sonia

    2015-09-10

    During last decades an increasing number of herbal products specifically targeting women's disorders has appeared in the worldwide marketplace. This growth highlights the need for a critical evaluation of quality, safety and efficacy of these products. Analytical techniques applied to the quality control of the main medicinal plants used for women health (relief of menopause and menstrual related symptoms) have been reviewed. Thanks to the innovation in analytical technology, identification and detection of secondary metabolites dramatically improved. In particular, hyphenated techniques have proved to be the most suitable for the rapid identification of compounds in plant matrix. Moreover, taking into account that differences in sample quality are not only found in the main compounds or in the chemical markers but also in the low-concentration compounds, fingerprint analysis might be a simple way for identification and quality control of herbal products containing a large number of low amounts of unknown compounds. Furthermore in several papers the informations obtained from the analysis of a plant have been processed by statistical elaborations. Medicinal plants here discussed are classified on the basis of the chemical markers used for their quality control. PMID:25863356

  12. The P450 superfamily: update on new sequences, gene mapping, and recommended nomenclature.

    Science.gov (United States)

    Nebert, D W; Nelson, D R; Coon, M J; Estabrook, R W; Feyereisen, R; Fujii-Kuriyama, Y; Gonzalez, F J; Guengerich, F P; Gunsalus, I C; Johnson, E F

    1991-01-01

    We provide here a list of 154 P450 genes and seven putative pseudogenes that have been characterized as of October 20, 1990. These genes have been described in a total of 23 eukaryotes (including nine mammalian and one plant species) and six prokaryotes. Of 27 gene families so far described, 10 exist in all mammals. These 10 families comprise 18 subfamilies, of which 16 and 14 have been mapped in the human and mouse genomes, respectively; to date, each subfamily appears to represent a cluster of tightly linked genes. We propose here a modest revision of the initially proposed (Nebert et al., DNA 6, 1-11, 1987) and updated (Nebert et al., DNA 8, 1-13, 1989) nomenclature system based on evolution of the superfamily. For the gene we recommend that the italicized root symbol CYP for human (Cyp for mouse), representing cytochrome P450, be followed by an Arabic number denoting the family, a letter designating the subfamily (when two or more exist), and an Arabic numeral representing the individual gene within the subfamily. A hyphen should precede the final number in mouse genes. We suggest that the human nomenclature system be used for other species. This system is consistent with our earlier proposed nomenclature for P450 of all eukaryotes and prokaryotes, except that we are discouraging the future use of cumbersome Roman numerals. PMID:1991046

  13. Square-Toed Boots and Felt Hats: Irish Revolutionaries and the Invasion of Canada (1848-1871

    Directory of Open Access Journals (Sweden)

    Marta Ramón-García

    2010-03-01

    Full Text Available The Fenian movement was born in 1858 as an alliance between the Irish Republican Brotherhood, a revolutionary secret society, and the Fenian Brotherhood, an Irish-American organisation intended to supply this society with funds and trained officers. This was not the first time that Irish nationalists on both sides of the Atlantic had tried to cooperate, but it was the first time that there was a steady arrangement in place. The Fenian partnership was extremely successful on the surface, but it was undermined by fundamental differences in customs, political attitudes and ultimate goals between Irish and American Fenians. The clearest evidence of these differences was afforded by the Fenian Brotherhood’s successive attempts to invade Canada between 1866 and 1871. As military episodes the Canadian raids were negligible; as Irish revolutionary attempts they seem absurd. However, they were a perfectly coherent manifestation of the Irish-American “hyphenated identity”. The present article traces the parallel evolution of the Irish Republican Brotherhood and the Fenian Brotherhood up to 1866, and reconstructs the cultural and political reasons for the revival of the Canadian scheme, the ensuing split in the Fenian Brotherhood, and the final collapse of the Fenian alliance.

  14. Sb(V reactivity with human blood components: redox effects.

    Directory of Open Access Journals (Sweden)

    Silvana López

    Full Text Available We assessed the reactivity of Sb(V in human blood. Sb(V reactivity was determined using an HPLC-HG-AFS hyphenated system. Sb(V was partially reduced to Sb(III in blood incubation experiments; however, Sb(III was a highly unstable species. The addition of 0.1 mol L(-1 EDTA prevented Sb(III oxidation, thus enabling the detection of the reduction of Sb(V to Sb(III. The transformation of Sb(V to Sb(III in human whole blood was assessed because the reduction of Sb(V in human blood may likely generate redox side effects. Our results indicate that glutathione was the reducing agent in this reaction and that Sb(V significantly decreased the GSH/GSSG ratio from 0.32 ± 0.09 to 0.07 ± 0.03. Moreover, the presence of 200 ng mL(-1 of Sb(V increased the activity of superoxide dismutase from 4.4 ± 0.1 to 7.0 ± 0.4 U mL(-1 and decreased the activity of glutathione peroxidase from 62 ± 1 to 34 ± 2 nmol min(-1 mL(-1.

  15. Extracellular synthesis of silver nanoparticles by novel Pseudomonas veronii AS41G inhabiting Annona squamosa L. and their bactericidal activity

    Science.gov (United States)

    Baker, Syed; Mohan Kumar, K.; Santosh, P.; Rakshith, D.; Satish, S.

    2015-02-01

    In present investigation extracellular synthesis of silver nanoparticles were synthesized using cell free supernatant of Pseudomonas veronii AS41G isolated from Annona squamosa L. The bacterium significantly reduced silver nitrate to generate silver nanoparticles which was characterized with hyphenated techniques. Synthesis of silver nanoparticles preliminary confirmed by UV-Visible spectrophotometry with the intense peak at 410 nm, Further FTIR analysis revealed the possible role of biomolecules in the supernatant responsible for mediating the nanoparticles formation. The XRD spectra exhibited the characteristic Bragg peaks of 1 0 0, 1 1 1, 2 0 0, and 2 2 0 facets of the face centred cubic symmetry of nanoparticles suggesting that these nanoparticles were crystalline in nature. TEM microgram showed polydispersity of nanoparticles with size ranging from 5 to 50 nm. Synthesized silver nanoparticles showed antibacterial activity against human and environmental pathogens including MRSA. The study enlightens the role of biosynthesized silver nanoparticles as an emerging alternative for drug resistant microorganisms. The obtained results are promising enough to pave the environmentally benign nanoparticle synthesis processes without use of any toxic chemicals and also envision the emerging role of endophytes towards synthesis of nanoparticles. With scanty reports available on P.veronii species, a new role has been reported in this study which will be very valuable for future researchers working on it.

  16. Qualitative and Quantitative Assessments of Aconiti Lateralis Radix Praeparata Using High-Performance Liquid Chromatography Coupled with Diode Array Detection and Hybrid Ion Trap-Time-of-Flight Mass Spectrometry.

    Science.gov (United States)

    Zhang, Na; Song, Yuelin; Song, Qingqing; Shi, Shepo; Zhang, Qian; Zhao, Yunfang; Li, Jun; Tu, Pengfei

    2016-07-01

    Dual roles have been widely disclosed for Aconiti Lateralis Radix Praeparata (Chinese name: Fuzi) by acting as an effective herbal medicine accompanied with high toxicity risk and narrow therapeutic range. Aconite alkaloids, also known as diterpenoid alkaloids (DAs), have been proved to be primary therapeutic as well as toxic material basis of Fuzi. In the present study, we aim to characterize qualitative profile along with quantitative features of DAs in Fuzi, which could benefit the quality control of Fuzi as well as its safe medication in clinic. Chromatographic fingerprinting was achieved using 12 batches of crude materials collected from different habitats (similarities >0.9) by hyphenating liquid chromatography (LC) with diode array detection. Simultaneous determination of six primary DAs, namely benzoylmesaconine, benzoylaconine, benzoylhypaconine, mesaconine, aconitine and hypaconitine, was also carried out. The developed method was systematically validated and successfully applied for quantitative characterization. Significant variations were observed regarding the contents of those six analytes among different raw materials. A total of 99 DAs were detected and characterized, including 9 unambiguous identities and 77 putative assignments, as well as 13 unknown compounds, from the representative extract by LC coupled with hybrid ion trap-time-of-flight mass spectrometry. The findings obtained herein could favor in-depth understanding of the chemical composition of DAs and the quality control of Fuzi.

  17. Chemical Characterization of Fruit Wine Made from Oblačinska Sour Cherry

    Directory of Open Access Journals (Sweden)

    Milica Pantelić

    2014-01-01

    Full Text Available This paper was aimed at characterizing the wine obtained from Oblačinska, a native sour cherry cultivar. To the best of our knowledge, this is the first paper with the most comprehensive information on chemical characterization of Oblačinska sour cherry wine. The chemical composition was characterized by hyphenated chromatographic methods and traditional analytical techniques. A total of 24 compounds were quantified using the available standards and another 22 phenolic compounds were identified based on the accurate mass spectrographic search. Values of total phenolics content, total anthocyanin content, and radical scavenging activity for cherry wine sample were 1.938 mg gallic acid eqv L−1, 0.113 mg cyanidin-3-glucoside L−1, and 34.56%, respectively. In general, cherry wine polyphenolics in terms of nonanthocyanins and anthocyanins were shown to be distinctive when compared to grape wines. Naringenin and apigenin were characteristic only for cherry wine, and seven anthocyanins were distinctive for cherry wine.

  18. Genuineness assessment of mandarin essential oils employing gas chromatography-combustion-isotope ratio MS (GC-C-IRMS).

    Science.gov (United States)

    Schipilliti, Luisa; Tranchida, Peter Quinto; Sciarrone, Danilo; Russo, Marina; Dugo, Paola; Dugo, Giovanni; Mondello, Luigi

    2010-03-01

    Cold-pressed mandarin essential oils are products of great economic importance in many parts of the world and are used in perfumery, as well as in food products. Reconstituted mandarin oils are easy to find on the market; useful information on essential oil authenticity, quality, extraction technique, geographic origin and biogenesis can be attained through high-resolution GC of the volatile fraction, or enantioselective GC, using different chiral stationary phases. Stable isotope ratio analysis has gained considerable interest for the unveiling of citrus oil adulteration, detecting small differences in the isotopic carbon composition and providing plenty of information concerning the discrimination among products of different geographical origin and the adulteration of natural essential oils with synthetic or natural compounds. In the present research, the authenticity of several mandarin essential oils was assessed through the employment of GC hyphenated to isotope ratio MS, conventional GC flame ionization detector, enantioselective GC and HPLC. Commercial mandarin oils and industrial natural (declared as such) mandarin essential oils, characterized by different harvest periods and geographic origins, were subjected to analysis. The results attained were compared with those of genuine cold-pressed Italian mandarin oils, obtained during the 2008-2009 harvest season. PMID:20112303

  19. Vitamin D-mediated modifications in protein-DNA interactions at two promoter elements of the osterocalcin gene

    International Nuclear Information System (INIS)

    By the combined use of DNase I footprinting, electrophoretic mobility-shift assay, and methylation interference analysis, the authors have identified a series of sequence-specific protein-DNA interactions in the 5' flanking region of the rat osteocalcin gene. Stimulation of osteocalcin gene expression by 1,25-dihydroxyvitamin D3, a physiologic mediator of this bone-specific gene in vitro and in vivo, is associated with modifications in the binding of ROS 17/2.8 cell nuclear factors to two promoter segments that up-regulate transcription. One segment located between -462 and -437 exhibits a vitamin D-dependent increase in sequence-specific binding of nuclear factors. This element (CTGGGTGAATGAGGACATTACT-GACC), identified at single nucleotide resolution, contains a region of hyphenated dyad symmetry and shares sequence homology with consensus steroid-responsive elements and with the sequence that has been identified as the vitamin D receptor binding site in the human osteocalcin gene. They have also observed that vitamin D stimulation of osteocalcin gene expression results in a 5-fold increase in protein binding to the region of the osteocalcin box, a 24-nucleotide segment in the proximal promoter with a CCAAT motif as the central core. The results demonstrate protein-DNA interactions in a vitamin D-responsive element and in a second sequence, the osteocalcin box, both of which are involved in the physiologic regulation of the osteocalcin gene in response to 1,25-dihydroxyvitamin D3