umu.sePublikasjoner
Endre søk
Begrens søket
1234 1 - 50 of 182
RefereraExporteraLink til resultatlisten
Permanent link
Referera
Referensformat
  • apa
  • ieee
  • modern-language-association-8th-edition
  • vancouver
  • Annet format
Fler format
Språk
  • de-DE
  • en-GB
  • en-US
  • fi-FI
  • nn-NO
  • nn-NB
  • sv-SE
  • Annet språk
Fler språk
Utmatningsformat
  • html
  • text
  • asciidoc
  • rtf
Treff pr side
  • 5
  • 10
  • 20
  • 50
  • 100
  • 250
Sortering
  • Standard (Relevans)
  • Forfatter A-Ø
  • Forfatter Ø-A
  • Tittel A-Ø
  • Tittel Ø-A
  • Type publikasjon A-Ø
  • Type publikasjon Ø-A
  • Eldste først
  • Nyeste først
  • Skapad (Eldste først)
  • Skapad (Nyeste først)
  • Senast uppdaterad (Eldste først)
  • Senast uppdaterad (Nyeste først)
  • Disputationsdatum (tidligste først)
  • Disputationsdatum (siste først)
  • Standard (Relevans)
  • Forfatter A-Ø
  • Forfatter Ø-A
  • Tittel A-Ø
  • Tittel Ø-A
  • Type publikasjon A-Ø
  • Type publikasjon Ø-A
  • Eldste først
  • Nyeste først
  • Skapad (Eldste først)
  • Skapad (Nyeste først)
  • Senast uppdaterad (Eldste først)
  • Senast uppdaterad (Nyeste først)
  • Disputationsdatum (tidligste først)
  • Disputationsdatum (siste først)
Merk
Maxantalet träffar du kan exportera från sökgränssnittet är 250. Vid större uttag använd dig av utsökningar.
  • 1. Ahlgren, Joakim
    et al.
    De Brabandere, Heidi
    Reitzel, Kasper
    Rydin, Emil
    Gogoll, Adolf
    Waldeback, Monica
    Sediment phosphorus extractants for phosphorus-31 nuclear magnetic resonance analysis: A quantitative evaluation2007Inngår i: Journal of Environmental Quality, ISSN 0047-2425, E-ISSN 1537-2537, Vol. 36, nr 3, s. 892-898Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    The influence of pre-extractant, extractant, and post-extractant on total extracted amounts of P and organic P compound groups measured with 31 P nuclear magnetic resonance (P-31-NMR) in lacustrine sediment was examined. The main extractants investigated were sodium hydroxide (NaOH) and sodium hydroxide ethylenediaminetetraacetic acid (NaOH-EDTA) with bicarbonate buffered dithionite (BD) or EDTA as pre-extractants. Post extractions were conducted using either NaOH or NaOH-EDTA, depending on the main extractant. Results showed that the most efficient combination of extractants for total P yield was NaOH with EDTA as pre-extractant, yielding almost 50% more than the second best procedure. The P compound groups varying the most between the different extraction procedures were polyphosphates and pyrophosphates. NaOH with BD as pre-extractant was the most efficient combination for these compound groups.

  • 2.
    Ahlgren, Ulf
    Umeå universitet, Medicinska fakulteten, Umeå centrum för molekylär medicin (UCMM).
    Imaging shows insulin-producing cells in diabetes2013Inngår i: TrAC. Trends in analytical chemistry, ISSN 0165-9936, E-ISSN 1879-3142, Vol. 44, s. III-IIIArtikkel i tidsskrift (Annet (populærvitenskap, debatt, mm))
  • 3.
    Alvarez, Laura
    et al.
    Umeå universitet, Medicinska fakulteten, Molekylär Infektionsmedicin, Sverige (MIMS). Umeå universitet, Medicinska fakulteten, Institutionen för molekylärbiologi (Medicinska fakulteten). Umeå universitet, Medicinska fakulteten, Umeå Centre for Microbial Research (UCMR).
    Hernandez, Sara B
    Umeå universitet, Medicinska fakulteten, Molekylär Infektionsmedicin, Sverige (MIMS). Umeå universitet, Medicinska fakulteten, Institutionen för molekylärbiologi (Medicinska fakulteten). Umeå universitet, Medicinska fakulteten, Umeå Centre for Microbial Research (UCMR).
    de Pedro, Miguel A
    Cava, Felipe
    Umeå universitet, Medicinska fakulteten, Molekylär Infektionsmedicin, Sverige (MIMS). Umeå universitet, Medicinska fakulteten, Institutionen för molekylärbiologi (Medicinska fakulteten). Umeå universitet, Medicinska fakulteten, Umeå Centre for Microbial Research (UCMR).
    Ultra-sensitive, high-resolution liquid chromatography methods for the high-throughput quantitative analysis of bacterial cell wall chemistry and structure2016Inngår i: Bacterial cell wall homeostasis: methods and protocols /edited by Hee-Jeon Hong / [ed] Hee-Jeon Hong, New York: Humana Press, 2016, Vol. 1440, s. 11-27Kapittel i bok, del av antologi (Fagfellevurdert)
    Abstract [en]

    High-performance liquid chromatography (HPLC) analysis has been critical for determining the structural and chemical complexity of the cell wall. However this method is very time consuming in terms of sample preparation and chromatographic separation. Here we describe (1) optimized methods for peptidoglycan isolation from both Gram-negative and Gram-positive bacteria that dramatically reduce the sample preparation time, and (2) the application of the fast and highly efficient ultra-performance liquid chromatography (UPLC) technology to muropeptide separation and quantification. The advances in both analytical instrumentation and stationary-phase chemistry have allowed for evolved protocols which cut run time from hours (2-3 h) to minutes (10-20 min), and sample demands by at least one order of magnitude. Furthermore, development of methods based on organic solvents permits in-line mass spectrometry (MS) of the UPLC-resolved muropeptides. Application of these technologies to high-throughput analysis will expedite the better understanding of the cell wall biology.

  • 4.
    Andersson, Patrik
    et al.
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Haglund, Peter
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Tysklind, Mats
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Ultraviolet absorption spectra of all 209 polychlorinated biphenyls evaluated by principal component analysis1997Inngår i: Fresenius' Journal of Analytical Chemistry, ISSN 0937-0633, E-ISSN 1432-1130, Vol. 357, nr 8, s. 1088-1092Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    The ultraviolet absorption spectra of all 209 polychlorinated biphenyls (PCBs) were recorded in the range 200-300 nm and displayed two important absorption maxima, viz., the main-band, lambda(max) 200-225 nm, and the kappa-band, lambda(max) 245-265 nm. By utilising principal component analysis, substitution related spectral characteristics of the PCBs, underlying the main patterns of the spectra, were examined. Captured in the multivariate evaluation were e.g., the importance of chlorine atoms in ortho positions, determining the intensity and existence of the kappa-band, chlorine substitution in para-para position, and the total number of chlorine atoms. The measured UV-spectra of all 209 polychlorinated biphenyls provide important physico-chemical descriptors for use in future quantitative structure-activity and structure-property relationship (QSAR/QSPR) studies.

  • 5.
    Appelblad, Patrik
    et al.
    Umeå universitet, Medicinska fakulteten, Institutionen för klinisk vetenskap. Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Jonsson, Tobias
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Bäckström, Torbjörn
    Umeå universitet, Medicinska fakulteten, Institutionen för klinisk vetenskap, Obstetrik och gynekologi.
    Irgum, Knut
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Determination of C-21 ketosteroids in serum using trifluoromethanesulfonic acid catalyzed precolumn dansylation and 1,1’-oxalyldiimidazole postcolumn peroxyoxalate chemiluminescence detection1998Inngår i: Analytical Chemistry, ISSN 0003-2700, E-ISSN 1520-6882, Vol. 70, nr 23, s. 5002-5009Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    A new procedure for the quantitation of C-21 ketosteroids using trifluoromethanesulfonic acid-catalyzed precolumn dansylation and coupled column liquid chromatographic separation, followed by postcolumn 1,1‘-oxalyldiimidazole peroxyoxalate chemiluminescence detection is presented. In the simultaneous optimization of chromatographic resolution and chemiluminescence intensity, a coupled column chromatographic system and a stopped-flow system were used. An eluent containing 20 mM phosphate buffer at pH 6.7 accomplished an efficient separation of 3α-hydroxy-5β-pregnan-20-one from a mixture containing 10 C-21 ketosteroids. Phosphate buffer also proved to be the most advantageous, among the six buffers tested, for sensitive detection. Experimental design and multivariate data analysis were used to characterize and optimize the postcolumn reaction chemistry in the chromatographic system. A valid full factorial design with excellent predictability showed that the flow rates for both 1,1‘-oxalyldiimidazole and hydrogen peroxide were the factors most strongly affecting the sensitivity of the system. The theoretical plate numbers were above 11 000 for all 10 dansylated ketosteroids. The 3σ detection limit estimated from 3α-hydroxy-5β-pregnan-20-one calibration curve data was 1.6 pmol (n = 4, 125 μL injected) and spiked serum containing 0−74 pmol of this compound showed overall recoveries of 73 ± 9% (n = 12). Quantitation of 3α-hydroxy-5β-pregnan-20-one was finally carried out on 45 serum samples and the results compared to those from a radioimmunoassay (RIA) method. The data acquired with the procedure described in this work compare well with the results from RIA, which confirms the reliability of the new analytical procedure.

  • 6. Appelblad, Patrik
    et al.
    Jonsson, Tobias
    Jiang, Wen
    Irgum, Knut
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Fast hydrophilic interaction liquid chromatographic separations on bonded zwitterionic stationary phase2008Inngår i: Journal of Separation Science, ISSN 1615-9306, E-ISSN 1615-9314, Vol. 31, nr 9, s. 1529-1536Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    Separation science is an art of obtaining adequate resolution of the desired compounds in minimum time, and with minimum effort in terms of sample preparation and data evaluation. In LC, where selectivity is a main driving force for separation, the availability of different separation modes capable of operating at high flow rates is a way to make combined optimal use of selectivity, efficiency, and speed. The separation of polar and hydrophilic compounds is problematic in RP LC due to the poor retention. Hydrophilic interaction liquid chromatography (HILIC) is a more straightforward separation mode to address this problem. Herein, it is shown that separations in HILIC mode are equally efficient as for RP, providing a potential for very fast separations on short columns. This is not only facilitated by the low viscosity of the mobile phase compositions used, compared to typical RP eluents, but also due to higher column permeability. To exemplify this, baseline separations of uracil and cytosine are shown in less than 4 s and of Tamiflu® and its main metabolite in less than 40 s, both under isocratic conditions. HILIC must therefore be considered having potential for high throughput purposes, and being an attractive candidate as the second separation dimension in 2-D HPLC.

  • 7. Arshadi, Mehrdad
    et al.
    Nilsson, Calle
    Magnusson, Bengt
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Gas chromatography-mass spectrometry determination of the pentafluorobenzoyl derivative of methylhydrazine in false morel (Gyromitra esculenta) as a monitor for the content of the toxin gyromitrin2006Inngår i: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1125, nr 2, s. 229-233Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    The main toxic compound found in false morel (Gyromitra esculenta) is acetaldehyde-N-methyl-N-formylhydrazone (gyromitrin). This paper describes a method of determining the total hydrazones content based on acid hydrolysis of gyromitrin and other related hydrazones in air-dried false morel followed by derivatisation of methylhydrazine with pentafluorobenzoyl chloride. The derivative, tris-pentafluorobenzoyl methylhydrazine (tris-PFB-MH) is analyzed by gas chromatography–mass spectrometry. The overall precision of the method is better than 10% (relative standard deviation) for 0.5 ng/μl methylhydrazine in solution. The minimum detectable concentration of methylhydrazine (tris-PFB-MH) by this method is estimated to be approximately 12 pg/μl, which is equal to 0.3 μg/g dry matter (DM) of false morel.

  • 8.
    Assefa, Anteneh
    et al.
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen. Dept. of Aquatic Sciences and Assessment, Swedish University of Agricultural Sciences (SLU), Uppsala, Sweden .
    Tysklind, Mats
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Klanova, Jana
    Wiberg, Karin
    Tracing the sources of PCDD/Fs in Baltic Sea air by using metals as source markers2018Inngår i: Environmental Science: Processes & Impacts, ISSN 2050-7887, E-ISSN 2050-7895, Vol. 20, nr 3, s. 544-552Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    The atmosphere is the major contributor of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) in the Baltic Sea environment. In this study, we investigated the potential of using metals along with PCDD/Fs as markers of important emission sources of PCDD/Fs in air. The air concentrations of PCDD/F congeners (n = 17), other persistent organic pollutants (n = 8) and metals (n = 16) were determined in summer and winter air using high volume samplers at a rural field station (Aspvreten, Sweden) located close to the Baltic Sea coast. During winter, PCDD/F levels were on average 20 times higher than in summer (5.1 +/- 5.8 fg toxicity equivalents (TEQ) m-3 and 0.26 +/- 0.18 fg TEQ m-3, respectively) mostly due to a higher fraction of PCDFs. The increased levels of PCDD/Fs were pronounced mainly in air masses that had travelled from southern (S) and eastern (E) compass sectors. A principal component analysis (PCA) of metal levels in Scots pine (Pinus sylvestris) needles sampled to reflect various air emission source types helped to identify potential marker metals for selected known atmospheric emission sources of PCDD/Fs and to rank among the candidate source types. Brown coal burning, domestic burning and heavy oil burning appeared to be the source types that contribute most of the PCDD/Fs in Baltic Sea air. The current study demonstrates a successful approach for source tracing of PCDD/Fs in air, where integrated indices from seasonal and spatial patterns of PCDD/Fs as well as metal source markers were used to trace and rank sources.

  • 9. Avagyan, Rozanna
    et al.
    Nyström, Robin
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Institutionen för tillämpad fysik och elektronik.
    Boman, Christoffer
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Institutionen för tillämpad fysik och elektronik.
    Westerholm, Roger
    Determination of hydroxylated polycyclic aromatic hydrocarbons by HPLC-photoionization tandem mass spectrometry in wood smoke particles and soil samples2015Inngår i: Analytical and Bioanalytical Chemistry, ISSN 1618-2642, E-ISSN 1618-2650, Vol. 407, nr 16, s. 4523-4534Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    A simple and fast method for analysis of hydroxylated polycyclic aromatic hydrocarbons using pressurized liquid extraction and high performance liquid chromatography utilizing photoionization tandem mass spectrometry was developed. Simultaneous separation and determination of nine hydroxylated polycyclic aromatic hydrocarbons and two hydroxy biphenyls could be performed in negative mode with a run time of 12 min, including equilibration in 5 min. The calibration curves were in two concentration ranges; 1-50 ng/mL and 0.01-50 mu g/mL, with coefficients of correlation R (2) > 0.997. The limits of detection and method quantification limits were in the range of 9-56 pg and 5-38 ng/g, respectively. A two-level full factorial experimental design was used for screening of conditions with the highest impact on the extraction. The extraction procedure was automated and suitable for a large number of samples. The extraction recoveries ranged from 70 to 102 % and the matrix effects were between 92 and 104 %. The overall method was demonstrated on wood smoke particles and soil samples with good analytical performance, and five OH-PAHs were determined in the concentration range of 0.19-210 mu g/g. As far as we know, hydroxylated polycyclic aromatic hydrocarbons were determined in wood smoke and soil samples using photoionization mass spectrometry for the first time in this present study. Accordingly, this study shows that high performance liquid chromatography photoionization tandem mass spectrometry can be a good option for the determination of hydroxylated polycyclic aromatic hydrocarbons in complex environmental samples.

  • 10. Axelsson, Sara
    et al.
    Eriksson, Kåre
    Umeå universitet, Medicinska fakulteten, Institutionen för folkhälsa och klinisk medicin, Yrkes- och miljömedicin.
    Nilsson, Ulrika
    Determination of resin acids during production of wood pellets-a comparison of HPLC/ESI-MS with the GC/FID MDHS 83/2 method2011Inngår i: Journal of Environmental Monitoring, ISSN 1464-0325, E-ISSN 1464-0333, Vol. 13, nr 10, s. 2940-2945Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    Resin acids are constituents of natural and technical products of widespread use. Exposure is known to cause health effects in the airways and on the skin. Liquid chromatography/positive ion electrospray-mass spectrometry (HPLC/pos ESI-MS) was investigated for determination of 7-oxodehydroabietic (7-OXO), dehydroabietic (DHAA) and abietic acid (AA) in wood dust-containing air samples as a derivatisation-free alternative to the GC/FID HSE method 83/2, developed by the Health and Safety Executive UK. The resin acid 7-OXO was measured as a marker for oxidised resin acids, which are known to be the main contact allergens in colophonium. The found detection limits were 0.42 ng m(-3) for 7-OXO, 5.2 ng m(-3) for DHAA and 9.4 ng m(-3) for AA, respectively, which are considerably lower than with the GC/FID method (24, 115 and 89 ng m(-3)). The two methods correlated well, although consistently and significantly lower concentrations of 7-OXO were detected with LC/MS. The higher concentration of this compound with MDHS 83/2 is suggested to be an artefact from the derivatisation step in the presence of soluble wood dust remains.

  • 11.
    Axner, Ove
    et al.
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Institutionen för fysik.
    Galbács, Gábor
    University of Szeged, Szeged, Hungary.
    Laser spectrometric techniques in analytical atomic spectrometry2012Inngår i: Encyclopedia of analytical chemistry, John Wiley & Sons, Ltd , 2012Kapittel i bok, del av antologi (Fagfellevurdert)
    Abstract [en]

    The main purpose of this article is to describe the theory, instrumentation, and analytical performance of laser analytical atomic spectrometry, focusing on absorption, fluorescence, and ionization techniques. The structure of the article is such that it first provides an outline of the theory of light-matter interactions that prevail for each type of technique as well as of the most common modulation techniques, primarily, wavelength modulation (WM). This is followed by a section that covers the most important types of instrumentation used. The article finally provides a detailed discussion on the specific instrumentation, mode of operation, use, performance, and applications (both analytical and diagnostic) of each technique. In terms of laser atomic absorption, the focus of the discussion is on the use of approaches to enhance the detection capability by either reducing the amount of noise (as is done by the wavelength modulation absorption spectrometry (WMAS) technique) or by providing an extended interaction length (giving rise to cavity-enhanced absorption spectrometry (CEAS) techniques in general, and cavity ring-down spectrometry (CRDS) in particular). Laser atomic fluorescence techniques (often referred to as laser-excited atomic fluorescence spectrometry (LEAFS)) as well as laser ionization techniques (termed either laser-enhanced ionization (LEI) or resonance ionization spectrometry (RIS)) are also covered in some detail. It is shown that several of these techniques are capable of detecting a variety of elements in liquid samples down to low picogram per milliliter (pg mL−1) or parts-per-trillion (ppt) concentrations and in low femtogram amounts. Also other properties of the techniques, e.g. selectivity and linear dynamic range (LDR), are in general superior to those of conventional (nonlaser-based techniques).

  • 12. Bergknut, Magnus
    et al.
    Persson, Per
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Skyllberg, Ulf
    Molecular characterization of brominated persistent pollutants using extended X-ray absorption fine structure (EXAFS) spectroscopy2008Inngår i: Analytical and Bioanalytical Chemistry, ISSN 1618-2642, E-ISSN 1618-2650, Vol. 390, nr 3, s. 921-928Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    X-ray absorption fine structure (EXAFS) spectroscopy spectra were collected for three brominated persistent pollutants: 6-bromo-2,4,5-trichlorophenol (BrTriClP), pentabromophenol (PentaBrP) and 3,3',5,5'-tetrabromobisphenol A (TBBA). The substances were selected to be symmetrical (BrTriClP and TBBA) or asymmetrical (PentaBrP) with respect to the atomic Br positions and to differ in the number of bromine and other halide atoms, as well as their relative positions. The asymmetrical PentaBrP was modelled with special detail as not all bromine atoms have identical coordination environments. The studied substances displayed unique EXAFS spectra, which could be used to determine the molecular structure in fair detail. We conclude that EXAFS spectroscopy is a suitable technique for molecular characterization of the comparatively complex molecules within the class of compounds of brominated organic persistent pollutants. A detailed understanding of the EXAFS spectra of the pure compounds opens up possibilities to study the interactions with soil and sediment matrices by means of EXAFS spectroscopy. Figure Brominated organic persistent pollutants are characterized by EXAFS spectroscopy.

  • 13.
    Blum, Kristin
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Targeted and untargeted analysis of organic contaminants from on-site sewage treatment facilities: Removal, fate and environmental impact2018Doktoravhandling, med artikler (Annet vitenskapelig)
    Abstract [en]

    On-site sewage treatment facilities (OSSFs) are widely used all over the world to treat wastewater when large-scale sewage treatment plants (STPs) are not economically feasible. Although there is great awareness that the release of untreated wastewater into the environment can lead to water-related diseases and eutrophication, little is known about organic contaminants and their removal by OSSFs, environmental load and fate. Thus, this PhD thesis aims to improve the knowledge about treatment efficiencies in current OSSFs, the environmental impact and fate of contaminants released from OSSFs, as well as how biochar fortification in sand filter (soil beds) OSSFs might increase removal of these contaminants. State-of-the-art analytical techniques for untargeted and targeted analyses were used and the results evaluated with univariate and multivariate statistics.

    Environmentally-relevant contaminants discharged from OSSFs were identified using untargeted analysis with two-dimensional gas chromatography mass spectrometry (GC×GC-MS) and a MS (NIST) library search in combination with a prioritization strategy based on environmental relevance. A method was successfully developed for the prioritized contaminants using solid phase extraction and GC×GC-MS, and the method was also applicable to untargeted analysis. This method was applied to several studies. The first study compared treatment efficiencies between STP and soil beds and showed that treatment efficiencies are similar or better in soil beds, but the removal among the same type of treatment facilities and contaminants varied considerably. Hydrophilic contaminants were generally inadequately removed in both types of treatment facilities and resulted in effluent levels in the nanogram per liter range.

    Additionally, several prioritized and sometimes badly removed compounds were found to be persistent, mobile, and bioavailable and two additional, untargeted contaminants identified by the NIST library search were potentially mobile. These contaminants were also found far from the main source, a large-scale STP, at Lake Ekoln, which is part of the drinking water reservoir Lake Mälaren, Sweden. The study also showed that two persistent, mobile and bioavailable contaminants were additionally bioaccumulating in perch. Sampling for this study was carried out over several seasons in the catchment of the River Fyris. Parts of this catchment were affected by OSSFs, other parts by STPs. Potential ecotoxicological risks at these sites were similar or higher at those affected by STPs compared to those affected by OSSFs. Mass fluxes per capita were calculated from these levels, which were higher at STP-affected than at OSSF-affected sites in summer and autumn, but not in winter. Possibly, the diffuse OSSF emissions occur at greater average distances from the sampling sites than the STP point emissions, and OSSF-affected sites may consequently be more influenced by fate processes.

    The studies carried out suggested that there is a need to improve current treatment technologies for the removal of hydrophilic contaminants. Thus, the final study of this thesis investigated char-fortified sand filters (soil beds) as potential upgrades for OSSFs using a combination of advanced chemical analysis and quantitative structure-property relationship modeling. Removal efficiencies were calculated from a large variety of contaminants that were identified by untargeted analysis using GC×GC-MS and liquid chromatography ion mobility mass spectrometry as well as library searches (NIST and Agilent libraries). On average, char-fortified sand filters removed contaminants better than sand, partly due to an enhanced removal of several hydrophilic contaminants with heteroatoms. After a two-year runtime, sorption and particularly biodegradation must have contributed to the removal of these compounds.

    Generally, the combination of targeted and untargeted analysis has proven valuable in detecting a large variety of organic contaminants, as well as unexpected ones. The results imply that OSSFs have similar or better removal efficiencies, similar or lower environmental risks and similar or lower mass fluxes per capita, compared to STPs. Biochar fortification can improve the removal of organic contaminants in soil beds, but further research is needed to find technologies that reduce the discharge of all types of organic contaminants.

  • 14.
    Blum, Kristin M.
    et al.
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen. Umeå University.
    Gallampois, Christine
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Andersson, Patrik L.
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Renman, G.
    Renman, A.
    Haglund, Peter
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Comprehensive assessment of organic contaminant removal from on-site sewage treatment facility effluent by char-fortified filter beds2019Inngår i: Journal of Hazardous Materials, ISSN 0304-3894, E-ISSN 1873-3336, Vol. 361, s. 111-122Artikkel i tidsskrift (Annet vitenskapelig)
    Abstract [en]

    The removal of organic contaminants from wastewater using cost-efficient and easily accessible methods have been increasingly studied in recent years. Most studies have focused on municipal sewage treatment plants; however, our study investigated treatment with char-fortified filter beds for on-site sewage treatment facilities (OSSFs). OSSFs are commonly used in rural and semi-urban areas all over the world to treat wastewater to reduce eutrophication and water-related diseases. To screen for a wide range of organic contaminants in order to improve the understanding of wastewater treatment efficiency and molecular properties, samples were taken from an OSSF field study site that used three filter types: sand, char-fortified sand, and char-fortified gas concrete. First, we screened for organic contaminants with state-of-the-art gas chromatography and liquid chromatography mass spectrometry-based targeted and untargeted analysis and then we developed quantitative structure-property relationship models to find the key molecular features responsible for the removal of organic contaminants. We identified 74 compounds, of which 24 were confirmed with reference standards. Amongst these 74 compounds were plasticizers, UV stabilizers, fragrances, pesticides, surfactant and polymer impurities, pharmaceuticals and their metabolites, and many biogenic compounds. Sand filters that are sometimes used as a last treatment step in OSSFs can remove hydrophobic contaminants. The addition of biochar significantly increases the removal of these and a few hydrophilic compounds (Wilcoxon signed-rank test, α = 0.05). Gas concrete did not appear to be suitable for the removal of organic contaminants. This study showed that, besides hydrophobic effects, biodegradation is the most important removal pathway in long-term field applications. However, further improvements are necessary to remove very hydrophilic contaminants as they were not removed with sand and biochar-fortified sand.

  • 15.
    Blum, Kristin M.
    et al.
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen. Umeå University.
    Haglund, Peter
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Gao, Qiuju
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Ahrens, L.
    Gros, M.
    Wiberg, K.
    Andersson, Patrik L.
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Mass fluxes per capita of organic contaminants from on-site sewage treatment facilities2018Inngår i: Chemosphere, ISSN 0045-6535, E-ISSN 1879-1298, nr 201, s. 864-873Artikkel i tidsskrift (Annet vitenskapelig)
    Abstract [en]

    This study is the first attempt to quantify environmental fluxes per capita of organic contaminants discharged from on-site sewage treatment facilities (OSSFs) in affected recipients. Five sites were monitored around the River Fyris in Sweden: three mainly affected by OSSFs and two mainly affected by municipal sewage treatment plants (STPs). Gas chromatography-mass spectrometry was used to determine environmental concentrations of 30 anthropogenic contaminants, including organophosphorus compounds, rubber and plastic additives, UV stabilizers, fragrances, surfactant ingredients and polycyclic aromatic hydrocarbons. Uni- and multivariate statistical analysis of the most frequently detected contaminants showed that median fluxes per capita of tris(1,3-dichloro-2-propyl) phosphate, tris(1-chloro-2-propyl) phosphate, tris(2-chloroethyl) phosphate, and n-butylbenzene sulfonamide were similar at OSSF and STP sites, but the mass fluxes per capita of tris-(2-butoxyethyl) phosphate, 2-(methylthio)benzothiazole, and galaxolide, were significantly lower (~2 to 3-fold) at OSSF sites than at STP sites (Mann-Whitney, α = 0.05). Differences between these sites were larger in samples collected in summer and autumn than in samples collected in winter. Deviations likely originated from differences in treatment technology and distances between source and sampling sites. Further studies are needed to characterize mass fluxes per capita of contaminants in waters that directly receive discharges from OSSFs.

  • 16.
    Bouchet, Sylvain
    et al.
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Björn, Erik
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Analytical developments for the determination of monomethylmercury complexes with low molecular mass thiols by reverse phase liquid chromatography hyphenated to inductively coupled plasma mass spectrometry2014Inngår i: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1339, s. 50-58Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    The behavior of monomethylmercury (MMHg) is markedly influenced by its distribution among complexes with low molecular mass (LMM) thiols but analytical methodologies dedicated to measure such complexes are very scarce up to date. In this work, we selected 15 LMM thiols often encountered in living organisms and/or in the environment and evaluated the separation of the 15 corresponding MMHg-thiol complexes by various high performance liquid chromatography (HPLC) columns. Two C18 (Phenomenex Synergi Hydro-RP and LunaC18(2)), two phenyl (Inertsil Ph 3 and 5 mu m) and one mixed-mode (Restek Ultra IBD) stationary phases were tested for their retention and resolution capacities of the various complexes. The objective was to find simple separation conditions with low organic contents in the mobile phase to provide optimal conditions for detection by inductively coupled plasma mass spectrometry (ICPMS). The 15 complexes were synthesized in solution and characterized by electrospray ionization-mass spectrometry (ESI-MS). The C18 columns tested were either not resolutive enough or too retentive. The 3 pm phenyl stationary phase was able to resolve 10 out of the 15 complexes in less than 25 min, under isocratic conditions. The mixed-mode column was especially effective at separating the most hydrophilic complexes (6 complexes out of the 15), corresponding to the main LMM thiols found in living organisms. The detection limits (DLs) for these two columns were in the low nanomolar range and overall slightly better for the phenyl column. The possibilities offered by such methodology were exemplified by monitoring the time-course concentrations of four MMHg-thiol complexes within a phytoplankton incubation containing MMHg in the presence of an excess of four added thiols. 

  • 17.
    Bruce, Stephen J
    et al.
    Umeå Plant Science Center, Department of Forest Genetics and Plant Physiology, Swedish University of Agricultural Sciences, Umeå, Sweden.
    Jonsson, Pär
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Antti, Henrik
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Cloarec, Olivier
    Technologie Servier, 45000 Orleans, France.
    Trygg, Johan
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Marklund, Stefan L
    Umeå universitet, Medicinska fakulteten, Institutionen för medicinsk biovetenskap, Klinisk kemi.
    Moritz, Thomas
    Umeå Plant Science Center, Department of Forest Genetics and Plant Physiology, Swedish University of Agricultural Sciences, Umeå, Sweden.
    Evaluation of a protocol for metabolic profiling studies on human blood plasma by combined ultra-performance liquid chromatography/mass spectrometry: From extraction to data analysis2009Inngår i: Analytical Biochemistry, ISSN 0003-2697, E-ISSN 1096-0309, Vol. 372, nr 2, s. 237-249Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    The investigation presented here describes a protocol designed to perform high-throughput metabolic profiling analysis on human blood plasma by ultra-performance liquid chromatography/mass spectrometry (UPLC/MS). To address whether a previous extraction protocol for gas chromatography (GC)/MS-based metabolic profiling of plasma could be used for UPLC/MS-based analysis, the original protocol was compared with similar methods for extraction of low-molecular-weight compounds from plasma via protein precipitation. Differences between extraction methods could be observed, but the previously published extraction method was considered the best. UPLC columns with three different stationary phases (C8, C18, and phenyl) were used in identical experimental runs consisting of a total of 60 injections of extracted male and female plasma samples. The C8 column was determined to be the best for metabolic profiling analysis on plasma. The acquired UPLC/MS data of extracted male and female plasma samples was subjected to principal component analysis (PCA) and orthogonal projections to latent structures discriminant analysis (OPLS–DA). Furthermore, a strategy for compound identification was applied here, demonstrating the strength of high-mass-accuracy time-of-flight (TOF)/MS analysis in metabolic profiling.

  • 18.
    Bui, Nhat Thi Hong
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Polyhydroxyl and Polyphosphorylcholine functionalized Silica for Hydrophilic interaction liquid Chromatography- Synthesis, characterization and application2012Doktoravhandling, med artikler (Annet vitenskapelig)
    Abstract [en]

    This thesis focuses on the development of new stationary phases for use in hydrophilic interaction liquid chromatography using TRIS-based and phosphorylcholine typed monomers and porous silica particles as starting substrates. In this thesis, several ways of polymerizing highly hydrophilic mono­mers onto pore surfaces of silica supports are described, based on several “grafting from” schemes. “Controlled/living” radical polymerizations including atom transfer radical polymerization (ATRP) and iniferter-mediated polymerization in conjunction with conventional free radical polymerization are demonstrated to be successful tools for grafting different hydrophilic monomers (polyhydroxyl and phosphorylcholine [meth]acrylamide/acrylates) onto the silica surfaces. Reaction solvents are proven to play an essential role to achieve efficient graft polymerization of activated silica surfaces with these amphiphilic vinylic monomers, which is difficult because of their restricted access to the activated surface in solvents that can be used because of solubility constraints.

    Two tentacle TRIS-based polymer grafted silica, namely TRIS-WAX – TRIS functionality bonded to silica via a C–N–C imine bond and TRIS-Amide – TRIS bonded to silica via an amide bond, prove to be useful as stationary phases for hydrophilic interaction chromatography (HILIC).The TRIS-WAX exhibits a mixed mode hydrophilic partitioning and weak anion exchange (HILIC/WAX) retention mechanism while retention by hydrophilic partitioning is the dominant mechanism on the neutral TRIS-Amide phase which lacks weak anion exchange (WAX) properties. Interestingly, both these phases have selectivities that are radically different from most commercial HILIC stationary phases.

    Finally, a method is demonstrated for synthesizing a stratified (graft-copolymerized) silica material based on N,N′-methylenebisacrylamide and 2-methacryloyloxyethyl phosphorylcholine (MPC) using a “controlled/living” photoiniferter-mediated polymerization from the N,N-diethyldithiocarbamate iniferter moiety immobilized silica surfaces. This polymerization method proves to be successful for graft-blockcopolymerization of different highly hydrophilic monomers onto the activated surfaces of porous silica. In this way, silica surfaces are grafted with a cross-linked amide-based hydrogel, on top of which a tentacle zwitterionic phosphorylcholine-typed layer is synthesized. The resulted material proves to be useful for HILIC separations and possesses different selectivity for the tested organic acids compared to that of commercial ZIC-cHILIC stationary phase.

  • 19. Butina, Karen
    et al.
    Loffler, Susanne
    Rhen, Mikael
    Umeå universitet, Medicinska fakulteten, Umeå Centre for Microbial Research (UCMR). Umeå universitet, Medicinska fakulteten, Molekylär Infektionsmedicin, Sverige (MIMS).
    Richter-Dahlfors, Agneta
    Electrochemical sensing of bacteria via secreted redox active compounds using conducting polymers2019Inngår i: Sensors and actuators. B, Chemical, ISSN 0925-4005, E-ISSN 1873-3077, Vol. 297, artikkel-id UNSP 126703Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    Bacterial infections and antibiotic resistance represent major global threats to public health. Current diagnostics use culture based assays that are reliable but slow, hence appealing for new rapid methods. Here we describe redox sensing as a novel concept for rapid, label-free detection of bacteria. We utilize a two-electrode poly(3,4-ethylenedioxythiophene):polystyrenesulfonate (PEDOT:PSS) based sensor for detection of bacterially secreted redox-active compounds. Using purified redox-active compounds, we show the ability of the sensor to detect and quantify compounds in micromolar concentrations within minutes. When applied for detection and quantification of Salmonella, we show that secreted, low molecular weight redox compounds cause reduction of the PEDOT:PSS electrode. A potential role of redox sensing in infection diagnostics was demonstrated as uropathogenic strains of E. coli., Staphylococcus, Enterococcus, Pseudomonas, Proteus, and Klebsiella spp., major causes of complicated urinary tract infections, were successfully detected in complex media or processed urine. Since numerous bacterial species are capable of extracellular electron transfer, redox sensing may find use as a generic method for bacterial detection with applications in research laboatories, the clinic and industry alike.

  • 20.
    Byström, Emil
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Porous polymeric materials for chromatography: Synthesis, functionalization and characterization2009Doktoravhandling, med artikler (Annet vitenskapelig)
    Abstract [en]

    Background: Separation science is heavily reliant on materials to fulfill ever more complicated demands raised by other areas of science, notably the rapidly expanding molecular biosciences and environmental monitoring. The key to successful separations lies in a combination of physical properties and surface chemistry of stationary phases used in liquid chromatographic separation, and this thesis address both aspects of novel separation materials.

    Methods: The thesis accounts for several approaches taken during the course of my graduate studies, and the main approaches have been i) to test a wild-grown variety of published methods for surface treatment of fused silica capillaries, to ascertain firm attachment of polymeric monoliths to the wall of microcolumns prepared in silica conduits; ii) developing a novel porogen scheme for organic monoliths including polymeric porogens and macromonomers; iii) evaluating a mesoporous styrenic monolith for characterization of telomers intended for use in surface modification schemes and; iv) to critically assess the validity of a common shortcut used for estimating the porosity of monoliths prepared in microconduits; and finally v) employing plasma chemistry for activating and subsequently modifying the surface of rigid, monodisperse particles prepared from divinylbenzene.

    Results: The efforts accounted for above have resulted in i) better knowledge of the etching and functionalization parameters that determine attachment of organic monoliths prepared by radical polymerization to the surface of silica; ii) polar methacrylic monoliths with a designed macroporosity that approaches the desired "connected rod" macropore morphology; iii) estab¬lishing the usefulness of monoliths prepared via nitroxide mediated polymerization in gradient polymer elution chromatography; iv) proving that scanning electron microscopy images are of limited value for assessing the macroporous properties of organic monoliths, and that pore measurements on externally polymerized monolith cocktails do not represent the porous properties of the same cocktail polymerized in narrow confinements; and v) showing that plasma bromination can be used as an activation step for rigid divinylbenzene particles to act as grafting handles for epoxy-containing telomers, that can be attached in a sufficiently dense layer and converted into carboxylate cation exchange layer that allows protein separations in fully aqueous eluents.

  • 21.
    Byström, Emil
    et al.
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Viklund, Camilla
    Merck SeQuant AB, Umeå.
    Irgum, Knut
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Differences in porous characteristics of styrenic monoliths prepared by controlled thermal polymerization in molds of varying dimensions2010Inngår i: Journal of Separation Science, ISSN 1615-9306, E-ISSN 1615-9314, Vol. 33, nr 2, s. 191-199Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    Nitroxide-mediated polymerization was used as a model system for preparing styrenic monolithic materials with significant mesopore contents in different mold formats, with the aim of assessing the validity of pore characterization of capillary monoliths by analysis of parallel bulk polymerized precursor solution. Capillary monoliths were prepared in 250 mm id fused silica tubes (quadruplicate samples, in total 17 m), and the batch polymerizations were carried out in parallel in 100 mL microvials and regular 2mL glass vials, both in quintuplicate. The monoliths recovered from the molds were characterized for their meso- and macroporous properties by nitrogen sorptiometry (three repeated runs on each sample), followed by a single analysis by mercury intrusion porosimetry. A total of 14 monolith samples were thus analyzed. A Grubbs’ test identified one regular vial sample as an outlier in the sorptiometric surface area measurements, and data from this sample were consequently excluded from the pore size calculations, which are based on the same nitrogen sorption data, and also from the mercury intrusion data set. The remaining data were subjected to single factor analyses of variance analyses to test if the porous properties of the capillary monoliths were different from those of the bulk monoliths prepared in parallel. Significant differences were found between all three formats both in their meso and macroporous properties. When the dimension was shrunk from conventional vial to capillary size, the specific surface area decreased from 52.274.7 to 34.671.7m2/g. This decrease in specific surface area was accompanied by a significant shift in median diameter of the through-pores, from 31073.9 to 544713 nm. None of these differences was obvious from the scanning electron micrographs that were acquired for each sample type. The common practice of determining the mesopore characteristics from analysis of samples prepared by parallel bulk polymerization and looking for changes in the macropore structure by visual assessment of SEMs are therefore both rather questionable, at least for monoliths of the kind used in this study.

  • 22.
    Carlsson, Sofia
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Installation of a hydride generation system coupled to atomic absorption spectrometry in Vientiene, Laos PDR - Determination of arsenic in water samples 2012Independent thesis Advanced level (degree of Master (One Year)), 20 poäng / 30 hpOppgave
    Abstract [en]

    Until now, the possibility for the personnel at the National University of Lao PDR (NUOL) to perform analysis of arsenic in drinking water as well as water used for agriculture has been limited to indication sticks, giving only a vague indication of the presence and levels of arsenic. Due to the lack of adequate and sensitive analytical instruments the levels of arsenic are relatively unknown in Lao People Democratic Republic (Lao PDR). A simple method of analyzing arsenic in water is using atomic absorption spectroscopy (AAS) coupled to a hydride generation system (HG). In support of this project, an HG with an AAS-oven has been delivered and installed at the inorganic lab at NUOL. The system has been optimized and tested and the personnel at the university have been instructed and trained in how to use the system. Sampling and analysis were supposed to be executed although this part of the project encountered many problems and could not be performed in a satisfactory way. Problems mainly came from lack of material, i.e. distilled water, and knowledge as well as monsoon weather conditions making the sampling impossible.

  • 23.
    Cedergren, Anders
    et al.
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Nordmark, Ulrika
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Determination of water in NIST reference material for mineral oils2000Inngår i: Analytical Chemistry, ISSN 0003-2700, E-ISSN 1520-6882, Vol. 72, nr 14, s. 3392-3395Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    The accuracy of the reference concentrations of moisture in electrical insulating oil RM 8506 and lubricating oil RM 8507 (both of mineral type) and specified by the National institute of Standards and Technology (NIST) as containing 39.7 and 76.8 ppm (w/w) water, respectively, has recently been the subject of debate in this journal. To shed some further light on this controversy, we report in this correspondence results for these oils obtained by two additional methods, one based on specially designed reagents for diaphragm-free Karl Fischer (KF) coulometry and the other based on the concept of stripping at elevated temperature/continuous KF coulometry. A positive interference effect was shown to take place for RM 8506 when the direct coulometric method was used. If the results are corrected for this, the values including six different procedures varied in the range 13.5-15.6 ppm (w/w). For RM 8507, all values were between 42.5 and 47.2 ppm (w/w), which means that the values recommended by NIST for both reference oils using volumetric titration are about twice as high as those obtained with the other techniques. A possible explanation for this discrepancy is presented.

  • 24. Chaintreau, Alain
    et al.
    Fieber, Wolfgang
    Sommer, Horst
    Gilbert, Alexis
    Yamada, Keita
    Yoshida, Naohiro
    Pagelot, Alain
    Moskau, Detlef
    Moreno, Aitor
    Schleucher, Jürgen
    Umeå universitet, Medicinska fakulteten, Institutionen för medicinsk kemi och biofysik.
    Reniero, Fabiano
    Holland, Margaret
    Guillou, Claude
    Silvestre, Virginie
    Akoka, Serge
    Remaud, Gerald S
    Site-specific C-13 content by quantitative isotopic C-13 nuclear magnetic resonance spectrometry: a pilot inter-laboratory study2013Inngår i: Analytica Chimica Acta, ISSN 0003-2670, E-ISSN 1873-4324, Vol. 788, s. 108-113Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    Isotopic C-13 NMR spectrometry, which is able to measure intra-molecular C-13 composition, is of emerging demand because of the new information provided by the C-13 site-specific content of a given molecule. A systematic evaluation of instrumental behaviour is of importance to envisage isotopic C-13 NMR as a routine tool. This paper describes the first collaborative study of intra-molecular C-13 composition by NMR. The main goals of the ring test were to establish intra-and inter-variability of the spectrometer response. Eight instruments with different configuration were retained for the exercise on the basis of a qualification test. Reproducibility at the natural abundance of isotopic C-13 NMR was then assessed on vanillin from three different origins associated with specific delta C-13(i) profiles. The standard deviation was, on average, between 0.9 and 1.2 parts per thousand for intra-variability. The highest standard deviation for inter-variability was 2.1%. This is significantly higher than the internal precision but could be considered good in respect of a first ring test on a new analytical method. The standard deviation of delta C-13(i) in vanillin was not homogeneous over the eight carbons, with no trend either for the carbon position or for the configuration of the spectrometer. However, since the repeatability for each instrument was satisfactory, correction factors for each carbon in vanillin could be calculated to harmonize the results.

    (C) 2013 Elsevier B.V. All rights reserved.

  • 25.
    Chen, Yang-Er
    et al.
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen. College of Life Sciences, Sichuan Agricultural University, Ya'an, China.
    Yuan, Shu
    Schröder, Wolfgang P.
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Comparison of methods for extracting thylakoid membranes of Arabidopsis plants2016Inngår i: Physiologia Plantarum: An International Journal for Plant Biology, ISSN 0031-9317, E-ISSN 1399-3054, Vol. 156, nr 1, s. 3-12Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    Robust and reproducible methods for extracting thylakoid membranes are required for the analysis of photosynthetic processes in higher plants such as Arabidopsis. Here, we compare three methods for thylakoid extraction using two different buffers. Method I involves homogenizing the plant material witha metal/glass blender; method II involves manually grinding the plant materialin ice-cold grinding buffer with a mortar and method III entails snap-freezing followed by manual grinding with a mortar, after which the frozen powder is thawed in isolation buffer. Thylakoid membrane samples extracted using each method were analyzed with respect to protein and chlorophyll content, yields relative to starting material, oxygen-evolving activity, protein complex content and phosphorylation. We also examined how the use of fresh and frozen thylakoid material affected the extracts’ contents of protein complexes. The use of different extraction buffers did not significantly alter the protein contentof the extracts in any case. Method I yielded thylakoid membranes with the highest purity and oxygen-evolving activity. Method III used low amounts of starting material and was capable of capturing rapid phosphorylation changes in the sample at the cost of higher levels of contamination. Method II yielded thylakoid membrane extracts with properties intermediate between those obtained with the other two methods. Finally, frozen and freshly isolated thylakoid membranes performed identically in blue native-polyacrylamide gel electrophoresis experiments conducted in order to separate multimeric protein supracomplexes.

  • 26.
    Claeson, Anna-Sara
    et al.
    Umeå universitet, Samhällsvetenskapliga fakulteten, Institutionen för psykologi.
    Gouveia-Figueira, Sandra C.
    Swedish Metabolomics Centre (SMC), Umeå, Sweden.
    Stenlund, Hans
    Swedish Metabolomics Centre (SMC), Umeå, Sweden.
    Johansson, Annika I.
    Swedish Metabolomics Centre (SMC), Umeå, Sweden.
    A standardized protocol for comparable analysis of GSH/GSSG by UHPLC-ESI-MSMS for human plasma2019Inngår i: Journal of chromatography. B, ISSN 1570-0232, E-ISSN 1873-376X, Vol. 1104, s. 67-72Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    Variability in the levels of GSH and GSSG in plasma is suggested to derive from inadequate pre-processing methods. The aim of this study was to develop a protocol for comparable and reliable measurements of GSH/GSSG. Venous blood from 8 healthy individuals were collected and divided into 7 different pre-processing procedures. For three of the samples an extraction mixture was added after 0 (baseline), 4 and 8 min and for three of the samples the extraction mixture was added at different times during defrost. A worst case scenario where a sample was left in a cool box during 6 h was also included. The samples were analyzed with UHPLC-ESIMSMS. A large difference in the levels of GSH and GSSG were identified and it was clearly associated with the sample handling procedures. A sample left untreated for 4 min will have significantly reduced amount of GSH. Stability tests showed that the level of GSH was reduced after 3 months in -80 degrees C.

  • 27.
    Courtois, Julien
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Monolithic separation media synthesized in capillaries and their applications for molecularly imprinted networks2006Doktoravhandling, med artikler (Annet vitenskapelig)
    Abstract [en]

    The thesis describes the synthesis of chromatographic media using several different approaches, their characterizations and applications in liquid chromatography. The steps to achieve a separation column for a specific analyte are presented. The main focus of the study was the design of novel molecularly imprinted polymers.

    Attachment of monolithic polymeric substrates to the walls of fused silica capillaries was studied in Paper I. With a broad literature survey, a set of common methods were tested by four techniques and ranked by their ability to improve anchoring of polymers. The best procedure was thus used for all further studies.

    Synthesis of monoliths in capillary columns was studied in Paper II. With the goal of separating proteins without denaturation, various monoliths were polymerized in situ using a set of common monomers and cross-linkers mixed with poly(ethylene glycol) as porogen. The resulting network was expected to present “protein-friendly pores”. Chemometrics were used to find and describe a set of co-porogens added to the polymerization cocktails in order to get good porosity and flow-through properties.

    Assessment of the macroporous structure of a monolith was described in Paper III. An alternative method to mercury intrusion porosimetry was proposed. The capillaries were embedded in a stained resin and observed under transmission electron microscope. Images were then computed to determine the pore sizes.

    Synthesis of molecularly imprinted polymers grafted to a core mono-lith in a capillary was described in Paper IV. The resulting material, imprinted with local anaesthetics, was tested for its chromatographic performance. Similar imprinted polymers were characterized by microcalorimetry in Paper V. Finally, imprinted monoliths were also synthesized in a glass tube and further introduced in a NMR rotor to describe the interactions between stationary phase and template in Paper VI.

  • 28. De Brabandere, Heidi
    et al.
    Danielsson, Rolf
    Sjoberg, Per J. R.
    Ahlgren, Joakim
    Rydin, Emil
    Waldeback, Monica
    Sediment extraction and clean-up for organic phosphorus analysis by electrospray ionization tandem mass spectrometry2008Inngår i: Talanta: The International Journal of Pure and Applied Analytical Chemistry, ISSN 0039-9140, E-ISSN 1873-3573, Vol. 74, nr 5, s. 1175-1183Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    A method to prepare NaOH sediment extracts for organic P compound analysis with electrospray ionization tandem mass spectrometry (ESI-MS-MS) was developed on natural samples. Ion exchange, rotary evaporation and mass cut-off filtering proved to be suitable for sample preparation. Samples were analyzed with ESI-MS-MS, and reproducibility and repeatability of the method was calculated. In addition, P-31-nuclear magnetic resonance Spectroscopy (P-31 NMR)was used to measure recovery of different P compound groups such as orthophosphate (Ortho-P), orthophosphate monoesters (Monoester-P), orthophosphate diesters (Diester-P) and pyrophosphates (Pyro-P). The developed sample preparation method resulted in an easy-to-spray liquid for the ESI-MS-MS instrumentation. The overall P recovery was 65% and P-31 NMR showed that Diester-P, possibly in the form of DNA, was apparently lost through the filtering step most likely due to their size. Variances in the total intensities of the MS scans (relative standard deviation (R.S.D.) 35-54%) were for about 50% due to repeated MS runs. Covariances of the peaks in the MS spectra were calculated to be for about 30% due to the sample preparation procedure. Finally, with the ESI-MS-MS approach, 11 peaks in the mass spectra were found likely to represent phosphate containing compounds. (c) 2007 Elsevier B.V. All rights reserved.

  • 29.
    Dinh, Ngoc Phuoc
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Investigations of the retention mechanisms in hydrophilic interaction chromatography2013Doktoravhandling, med artikler (Annet vitenskapelig)
    Abstract [en]

    Hydrophilic interaction chromatography is well known as a powerful technique separation of polar and ionizable compound nowadays. However the retention mechanism of the technique is still under debate. Understanding retention mechanism would facilitate the method development using the technique and its future improvement. This was inspiring and became the goal of this thesis.

    This work involves the characterization of the water enriched layer regarding to water and buffer salt accumulation. Twelve HILIC stationary phase with a diverse surface chemistry regarding to function groups and modification type were studied. Effect of water and salt on regarding to the retention mechanism was investigated by correlating the adsorption data to the retention of selected solutes

    This also involved the characterization of interactions involve in the separation of 21 HILIC columns. Interactions was probe by retention ratio of pair solutes which are characteristic for each specific interaction. The data was evaluate using principle component analysis – a multivariable data analysis method. The model was comprehensive and its outcomes were confirmed by the studies on adsorptions of water and salts.

  • 30.
    Dinh, Ngoc Phuoc
    et al.
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Jonsson, Tobias
    Merck SeQuant AB, S-90719 Umeå, Sweden.
    Irgum, Knut
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Accumlations of ammonium acetate on polar materials under HILIC condition and its relation to retention of analytesManuskript (preprint) (Annet vitenskapelig)
    Abstract [en]

    Ammonium acetate is a buffer salt commonly added to mobile phase in HILIC to improve the reproducibility of the retention of analytes. Adding buffer salt would then result to the change in retention and selectivity. In this study, we have developed methods for determine ammonium acetate in form of its hydrolyzed products (ammonium ion and acetate ion) adsorption on twelve different HILIC stationary phases under various mobile phase condition. The effect of functional group and mobile phase compositions on salt adsorption was then discussed. We also tried to develop a method for characterization important retention mechanism of HILIC systems and interpreted them under the relationship with salt adsorption. Adsorption of salt was based on both portioning and electrostatic interaction. Ammonium was found to preferentially adsorb on HILIC stationary phases except Purospher Star NH2 phase. It is worth noting that adding salt to mobile phase can promote partitioning retention mechanism, possibly as a result of phase separation due to salt out effect.

  • 31.
    Dinh, Ngoc Phuoc
    et al.
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen. Merck SeQuant AB, Umeå.
    Jonsson, Tobias
    Merck SeQuant AB, Umeå.
    Irgum, Knut
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Water uptake on polar stationary phases under conditions for hydrophilic interaction chromatography and its relation to solute retention2013Inngår i: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1320, s. 33-47Artikkel i tidsskrift (Annet vitenskapelig)
    Abstract [en]

    In hydrophilic interaction chromatography, water is known to accumulate on the stationary phase to form a water enriched layer, which is believed to play an important role in the retention mechanism. To gain a better understanding retention mechanism in HILIC, we have determined the water uptake on twelve different HILIC stationary phases. Non-modified and monomerically functionalized silica phases followed a pattern of monolayer formation followed by multiple layer adsorption, while the water uptake on polymerically functionalized silica stationary phase showed the characteristics of formation and swelling of hydrogels. This difference in the nature of water accumulation was found to be related to different water uptake patterns when methanol and tetrahydrofuran were added to 80:20 % (v/v) acetonitrile/water by replacing 5 % of the acetonitrile as tertiary solvents, and also when ammonium acetate was added as buffering electrolyte. The relationship between water uptake and retention mechanism was investigated by looking at the correlation between retention factors of neutral analytes and phase ratios of HILIC columns, calculated either as surface area (adsorption) or volume of the water layer enriched from the acetonitrile/water eluent (partitioning). Regardless of the adsorption or partitioning mechanism, the interaction of neutral analytes and stationary phase could be mainly the hydrogen bonding between analytes and the accumulated water in the water enriched layer.

  • 32.
    Dinh, Ngoc Phuoc
    et al.
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Nguyen, Anh Mai
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Quach, Minh Cam
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Shchukarev, Andrei
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Irgum, Knut
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Functionalization of epoxy-based monoliths for ion exchange chromatography of proteins2009Inngår i: Journal of Separation Science, Vol. 32, nr 15-16, s. 2556-2564Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    Macroporous epoxy-based monoliths prepared by emulsion polymerization have been modified for use in ion exchange chromatography (IEC) of proteins. Strong anion exchange functionality was established by iodomethane quaternization of tertiary amine present on the monolith surface as a part of the polymer backbone. The modification pathway to cation exchange materials was via incorporation of glycidyl methacrylate (GMA) brushes which were coated using atom transfer radical polymerization (ATRP). Strong (SO3-) and weak (COO-) cation exchange groups were thereafter introduced onto the GMA-grafted monoliths by reactions with sodium hydrogen sulfite and iminodiacetic acid, respectively. Grafting was confirmed by XPS, gravimetric measurement, and chromatographic behavior of the modified materials toward model proteins. In incubation experiments the proteins were recovered quantitatively with no obvious signs of unfolding after contact with the stationary phase for >2 h. Chromatographic assessments on the functionalized columns as well as problems associated with flow-through modification by ATRP are discussed.

  • 33.
    Do, Lan
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    New tools for sample preparation and instrumental analysis of dioxins in environmental samples2013Doktoravhandling, med artikler (Annet vitenskapelig)
    Abstract [en]

    Polychlorinated dibenzo-p-dioxins (PCDDs) and dibenzofurans (PCDFs), two groups of structurally related chlorinated aromatic hydrocarbons, are of high concern due to their global distribution and extreme toxicity. Since they occur at very low levels, their analysis is complex, challenging and hence there is a need for efficient, reliable and rapid alternative analytical methods. Developing such methods was the aim of the project this thesis is based upon.

    During the first years of the project the focus was on the first parts of the analytical chain (extraction and clean-up). A selective pressurized liquid extraction (SPLE) procedure was developed, involving in-cell clean-up to remove bulk co-extracted matrix components from sample extracts. It was further streamlined by employing a modular pressurized liquid extraction (M-PLE) system, which simultaneously extracts, cleans up and isolates planar PCDD/Fs in a single step. Both methods were validated using a wide range of soil, sediment and sludge reference materials. Using dichloromethane/n-heptane (DCM/Hp; 1/1, v/v) as a solvent, results statistically equivalent to or higher than the reference values were obtained, while an alternative, less harmful non-chlorinated solvent mixture - diethyl ether/n-heptane (DEE/Hp; 1/2, v/v) – yielded data equivalent to those values.

    Later, the focus of the work shifted to the final instrumental analysis. Six gas chromatography (GC) phases were evaluated with respect to their chromatographic separation of not just the 17 most toxic congeners (2,3,7,8-substituted PCDD/Fs), but all 136 tetra- to octaCDD/Fs. Three novel ionic liquid columns performed much better than previously tested commercially available columns. Supelco SLB-IL61 offered the best overall performance, successfully resolving 106 out of the 136 compounds, and 16 out of the 17 2,3,7,8-substituted PCDD/Fs. Another ionic liquid (SLB-IL111) column provided complementary separation. Together, the two columns separated 128 congeners. The work also included characterization of 22 GC columns’ selectivity and solute-stationary phase interactions. The selectivities were mapped using Principal Component Analysis (PCA) of all 136 PCDD/F’s retention times on the columns, while the interactions were probed by analyzing both the retention times and the substances’ physicochemical properties.

  • 34.
    Do, Lan
    et al.
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Lundstedt, Staffan
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Haglund, Peter
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Optimization of selective pressurized liquid extraction for extraction and in-cell clean-up of PCDD/Fs in soils and sediments2013Inngår i: Chemosphere, ISSN 0045-6535, E-ISSN 1879-1298, Vol. 90, nr 9, s. 2414-2419Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    This paper describes the development of methods for selective extraction of polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) from soils and sediments, using pressurized liquid extraction with in-cell clean-up (SPLE). Two binary solvent mixtures, viz. dichloromethane/n-heptane (DCM/Hp), and diethylether/n-heptane (DEE/Hp), were evaluated. The SPLE extraction conditions were optimized using central composite face (CCF) design. Three factors were investigated: extraction temperature (60-160°C), number of extraction cycles (1-3) and time per cycle (2-18min). The results showed that DCM/Hp (1/1, v/v) and DEE/Hp (1/2, v/v) were the best extraction solvent compositions and that the extraction temperature was a critical factor that needed careful optimization to achieve high extraction efficiency without co-extraction of sulfuric acid. Under the optimal conditions, the SPLE methods provided results with good accuracy and precision. For the sandy soil certified reference material (CRM-529) the quantification results ended up in the range 82-110% as compared to the concentrations obtained by a reference method based on Soxhlet extraction and external column clean-up. Furthermore, for a clay soil (CRM-530) and a sediment reference material (WMS-01), the accuracy (trueness) of the TEQ values were +11% (DCM/Hp) and +8% (DEE/Hp) for CRM-530, +8% and -7% for WMS-01, respectively. The individual congener concentrations also agreed well with the certified values. These findings show that SPLE is a promising method for combined extraction and clean-up of PCDD/Fs in soil/sediment samples.

  • 35.
    Do, Lan
    et al.
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Xuan, Thong H.
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Lundstedt, Staffan
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Haglund, Peter
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Modular pressurized liquid extraction for simultaneous extraction, clean-up and fractionation of PCDD/Fs in soil, sediment and sludge samples2013Inngår i: Analytical Methods, ISSN 1759-9660, E-ISSN 1759-9679, nr 5, s. 1231-1237Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    Modular pressurized liquid extraction (M-PLE) procedures were developed for simultaneous extraction, clean-up and fractionation of polychlorinated dioxins and furans (PCDD/Fs) in soil, sediment and sludge samples. The procedures utilize two coupled extraction cells: an upstream cell filled with the sample and layers of silica and acid- and base-modified silica, and a downstream cell filled with activated carbon. The silica layers were added to remove polar or hydrolysable matrix components, and the carbon to perform planarity-based fractionation. Two solvent systems (dichloromethane–heptane, DCM–Hp and diethyl ether–heptane, DEE–Hp) and two activated carbon loads (1% and 3% carbon on Celite) were evaluated using certified reference materials (CRM-529 and WMS-01) and materials from previous inter-calibration studies. Using any of the four procedures, data statistically equivalent to the certified or reference values were obtained. The M-PLE procedure using DCM–Hp and 1% carbon sometimes extracted the reference materials more efficiently than the reference methods, while the DEE–Hp procedure extracted them equally efficient, offering an alternative with less environmental impact. The methods with 1% carbon on Celite produced sufficiently pure extracts for sample loads up to one gram, but for greater sample loads the higher carbon load (3% carbon on Celite) was required to avoid breakthrough of target analytes. The new streamlined procedures are fast, cost-efficient, involve relatively low environmental impact (in the case of DEE–Hp) and are well suited for high-throughput analysis of solid samples, e.g. in connection with environmental monitoring campaigns and major soil remediation efforts.

  • 36.
    Elhaj, Ahmed
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Porous Polymeric Monoliths by Less Common Pathways: Preparation and Characterization2014Doktoravhandling, med artikler (Annet vitenskapelig)
    Abstract [en]

    This thesis focuses on my endeavors to prepare new porous polymeric monoliths that are viable to use as supports in flow-through processes. Polymer monoliths of various porous properties and different chemical properties have been prepared utilizing the thermally induced phase separation (TIPS) phenomenon and step-growth polymerization reactions. The aim has been to find appropriate synthesis routes to produce separation supports with fully controlled chemical, physical and surface properties. This thesis includes preparation of porous monolithic materials from several non-cross-linked commodity polymers and engineering plastics by dissolution/precipitation process (i.e. TIPS). Elevated temperatures, above the upper critical solution temperature (UCST), were used to dissolve the polymers in appropriate solvents that only dissolve the polymers above this critical temperature. After dissolution, the homogeneous and clear polymer-solvent solution is thermally quenched by cooling. A porous material, of three dimensional structure, is then obtained as the temperature crosses the UCST. More than 20 organic solvents were tested to find the most compatible one that can dissolve the polymer above the UCST and precipitate it back when the temperature is lowered. The effect of using a mixture of two solvents or additives (co-porogenic polymer or surfactant) in the polymer dissolution/precipitation process have been studied more in depth for poly(vinylidine difluoride) (PVDF) polymers of two different molecular weight grades. Monolithic materials showing different pore characteristics could be obtained by varying the composition of the PVDF-solvent mixture during the dissolute­ion/precipitation process. Step-growth polymerization (often called polycondensat­ion reaction) combined with sol-gel process with the aid of porogenic polymer and block copolymer surfactant have also been used as a new route of synthesis for production of porous melamine-formaldehyde (MF) monoliths. In general, the meso- and macro-porous support materials, for which the synthesis/preparation is discussed in this thesis, are useful to a wide variety of applications in separation science and heterogeneous reactions (catalysis).

  • 37. Eriksson, Lennart
    et al.
    Trygg, Johan
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Wold, Svante
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen. Umetrics Inc., 42 Pine Hill Rd, Hollis, NH 03049, USA.
    PLS-trees (R), a top-down clustering approach2009Inngår i: Journal of Chemometrics, ISSN 0886-9383, E-ISSN 1099-128X, Vol. 23, nr 11, s. 569-580Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    A hierarchical clustering approach based on a set of PLS models is presented. Called PLS-Trees (R), this approach is analogous to classification and regression trees (CART), but uses the scores of PLS regression models as the basis for splitting the clusters, instead of the individual X-variables. The split of one cluster into two is made along the sorted first X-score (t(1)) of a PLS model of the cluster, but may potentially be made along a direction corresponding to a combination of scores. The position of the split is selected according to the improvement of a weighted combination of (a) the variance of the X-score, (b) the variance of Y and (c) a penalty function discouraging an unbalanced split with very different numbers of observations. Cross-validation is used to terminate the branches of the tree, and to determine the number of components of each cluster PLS model. Some obvious extensions of the approach to OPLS-Trees and trees based on hierarchical PLS or OPLS models with the variables divided in blocks depending on their type, are also mentioned. The possibility to greatly reduce the number of variables in each PLS model on the basis of their PLS w-coefficients is also pointed out. The approach is illustrated by means of three examples. The first two examples are quantitative structure-activity relationship (QSAR) data sets, while the third is based on hyperspectral images of liver tissue for identifying different sources of variability in the liver samples.

  • 38. Evertsson, Emma
    et al.
    Rönnberg, Julia
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Stalring, Jonna
    Thunberg, Linda
    A hierarchical screening approach to enantiomeric separation2017Inngår i: Chirality, ISSN 0899-0042, E-ISSN 1520-636X, Vol. 29, nr 5, s. 202-212Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    The screening of a number of chiral stationary phases (CSPs) with different modifiers in supercritical fluid chromatography to find a chromatographic method for separation of enantiomers can be time-consuming. Computational methods for data analysis were utilized to establish a hierarchical screening strategy, using a dataset of 110 drug-like chiral compounds with diverse structures tested on 15 CSPs with two different modifiers. This dataset was analyzed using a combinatorial algorithm, principal component analysis (PCA), and a correlation matrix. The primary goal was to find a set of eight columns resolving a large number of compounds, but also having complementary enantioselective properties. In addition to the hereby defined hierarchical experimental strategy, quantitative structure enantioselective models (QSERs) were evaluated. The diverse chemical space and relatively limited size of the training set reduced the accuracy of the QSERs. However, including separation factors from other CSPs increased the accuracies of the QSERs substantially. Hence, such combined models can support the experimental strategy in prioritizing the CSPs of the second screening phase, when a compound is not separated by the primary set of columns.

  • 39.
    Fahlman, Johan
    et al.
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Institutionen för ekologi, miljö och geovetenskap.
    Fick, Jerker
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Karlsson, Jan
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Institutionen för ekologi, miljö och geovetenskap.
    Jonsson, Micael
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Institutionen för ekologi, miljö och geovetenskap.
    Brodin, Tomas
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Institutionen för ekologi, miljö och geovetenskap. Department of Wildlife, Fish, and Environmental Studies, Swedish University of Agricultural Sciences, Umeå, Sweden.
    Klaminder, Jonatan
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Institutionen för ekologi, miljö och geovetenskap.
    Using laboratory incubations to predict the fate of pharmaceuticals in aquatic ecosystems2018Inngår i: Environmental Chemistry, ISSN 1448-2517, E-ISSN 1449-8979, Vol. 15, nr 8, s. 463-471Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    Environmental contextEnvironmental persistence of excreted pharmaceuticals in aquatic ecosystems is usually predicted using small-scale laboratory experiments assumed to simulate natural conditions. We studied five pharmaceuticals comparing their removal rates from water under laboratory conditions and under natural environmental conditions existing in a large pond. We found that the laboratory conditions did not fully capture the complexity within the pond, which led to different removal rates in the two systems. AbstractEnvironmental persistence is a key property when evaluating risks with excreted pharmaceuticals in aquatic ecosystems. Such persistence is typically predicted using small-scale laboratory incubations, but the variation in aquatic environments and scarcity of field studies to verify laboratory-based persistence estimates create uncertainties around the predictive power of these incubations. In this study we: (1) assess the persistence of five pharmaceuticals (diclofenac, diphenhydramine, hydroxyzine, trimethoprim and oxazepam) in laboratory experiments under different environmental conditions; and (2) use a three-month-long field study in an aquatic ecosystem to verify the laboratory-based persistence estimates. In our laboratory assays, we found that water temperature (TEMP), concentrations of organic solutes (TOC), presence of sediment (SED), and solar radiation (SOL) individually affected dissipation rates. Moreover, we identified rarely studied interaction effects between the treatments (i.e. SOLxSED and TEMPxSOL), which affected the persistence of the studied drugs. Half-lives obtained from the laboratory assays largely explained the dissipation rates during the first week of the field study. However, none of the applied models could accurately predict the long-term dissipation rates (month time-scale) from the water column. For example, the studied antibioticum (trimethoprim) and the anti-anxiety drug (oxazepam) remained at detectable levels in the aquatic environment long after (similar to 150 days) our laboratory based models predicted complete dissipation. We conclude that small-scale laboratory incubations seem sufficient to approximate the short-term (i.e. within a week) dissipation rate of drugs in aquatic ecosystems. However, this simplistic approach does not capture interacting environmental processes that preserve a fraction of the dissolved pharmaceuticals for months in natural water bodies.

  • 40. Fick, J.
    et al.
    Pommer, L.
    Andersson, B.
    Nilsson, C.
    Experimental design as a tool to study gas-phase reactions in ventilation ducts2002Konferansepaper (Fagfellevurdert)
  • 41.
    Galindo-Prieto, Beatriz
    et al.
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Eriksson, Lennart
    MKS Umetrics, Umeå, Sweden.
    Trygg, Johan
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Variable influence on projection (VIP) for orthogonal projections to latent structures (OPLS)2014Inngår i: Journal of Chemometrics, ISSN 0886-9383, E-ISSN 1099-128X, Vol. 28, nr 8, s. 623-632Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    A new approach for variable influence on projection (VIP) is described, which takes full advantage of the orthogonal projections to latent structures (OPLS) model formalism for enhanced model interpretability. This means that it will include not only the predictive components in OPLS but also the orthogonal components. Four variants of variable influence on projection (VIP) adapted to OPLS have been developed, tested and compared using three different data sets, one synthetic with known properties and two real-world cases.

  • 42.
    Goitom Asfaha, Daniel
    Umeå universitet, Teknisk-naturvetenskaplig fakultet, Kemi.
    Fundamental Studies on Direct Injection Nebulisers for Sample Introduction in ICP Spectrometry: Aerosol Properties, ICP Characteristics and Analytical Performance2006Doktoravhandling, med artikler (Annet vitenskapelig)
    Abstract [en]

    The performance of different types of nebulisers: Vulkan direct injection nebuliser (Vulkan DIN), direct injection high efficiency nebuliser (DIHEN), microconcentric nebuliser coupled to cyclonic or double pass spray chamber (MCN-C or MCN-DP, respectively) was investigated and compared when used for sample introduction to ICP-MS or ICP-OES. With ICP-OES, in axial viewing mode, intensity distributions across the radius of the plasma (radial intensity profiles) were determined for different spectral lines with Esum 1.85-15.41 eV to determine fundamental plasma properties for various matrices using Vulkan DIN and MCN-C. The results showed that with the MCN-C the ionisation temperature (Tion) was about the same across the measured region of the plasma (±3.0 mm) whereas with the Vulkan DIN the Tion was significantly lower in the centre of the plasma. A large deviation from local thermodynamic equilibrium, as well as deteriorated stability, was observed for the plasma when using the Vulkan DIN.

    With ICP-MS noise power spectra (NPS) were generated to identify sources of noise. NPS showed that the magnitude of white noise for the tested sample introduction systems decreased in the following order: Vulkan DIN > DIHEN > MCN-C > MCN-DP. This order follows the decrease of mean droplet size and span of the size distribution, indicating that the white noise is caused by spatial and temporal non-uniform desolvation and ionisation. Another source of noise arose from the peristaltic pump and the magnitude of pump interference noise decreased in the following order: DIHEN > MCN-C/DP > Vulkan DIN. Mains power interference noise and 1/f noise were lower for the direct injection nebulisers compared to the spray chamber systems. The contribution or effects of these noise components on relative standard deviations of steady-state ion-count rate and isotope ratio measurements is discussed in this thesis.

    Aerosols generated by the Vulkan DIN and the DIHEN were also directly characterised using Particle Dynamic Analysis. The Vulkan DIN produced particles with a mean diameter of ~30 µm and a size distribution between 2-80 µm. With the DIHEN the corresponding values were ~11 µm and 1-40 µm, respectively, with a few particles at 55-78 µm. The mean velocity of particles from the Vulkan DIN was ~10 m s-1 and from the DIHEN ~18 m s-1. The lower velocity allows longer residence time counteracting the effects of the larger droplet size.

  • 43. Grabicova, Katerina
    et al.
    Grabic, Roman
    Fedorova, Ganna
    Fick, Jerker
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Cerveny, Daniel
    Kolarova, Jitka
    Turek, Jan
    Zlabek, Vladimir
    Randak, Tomas
    Bioaccumulation of psychoactive pharmaceuticals in fish in an effluent dominated stream2017Inngår i: Water Research, ISSN 0043-1354, E-ISSN 1879-2448, Vol. 124, s. 654-662Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    The treated effluent from sewage treatment plants (STP) is a major source of active pharmaceutical ingredients (APIs) that enter the aquatic environment. Bioaccumulation of 11 selected psychoactive pharmaceuticals (citalopram, clomipramine, haloperidol, hydroxyzine, levomepromazine, mianserin, mirtazapine, paroxetine, sertraline, tramadol and venlafaxine) was examined in Zivny Stream (tributary of the Blanice River, the Czech Republic), which is a small stream highly affected by effluent from the Prachatice STP. Six of the 11 pharmaceuticals were detected in grab water samples and in passive samplers. All pharmaceuticals were found in fish exposed to the stream for a defined time. The organs with highest presence of the selected pharmaceuticals were the liver and kidney; whereas only one pharmaceutical (sertraline) was detected in the brain of exposed fish. Fish plasma and muscle samples were not adequate in revealing exposure because the number of hits was much lower than that in the liver or kidney. Using the criterion of a bioaccumulation factor (BAF) >= 500, citalopram, mianserin, mirtazapine and sertraline could be classified as potential bioaccumulative compounds. In combination, data from integrative passive samplers and fish liver or kidney tissue samples were complimentary in detection of target compounds and simultaneously helped to distinguish between bioconcentration and bioaccumulation.

  • 44.
    Haglund, Peter
    et al.
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Korytár, Peter
    Danielsson, Conny
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Diaz, Jordí
    Wiberg, Karin
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Leonards, Pim
    Brinkman, Udo
    de Boer, Jacob
    GCxGC-ECD a promising method for the determination of dioxins and dioxin-like PCBs in food and feed2008Inngår i: Analytical and Bioanalytical Chemistry, ISSN 1618-2642, E-ISSN 1618-2650, Vol. 390, nr 7, s. 1815-1827Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    There is a need for cost-efficient alternatives to gas chromatography (GC)–high-resolution mass spectrometry (HRMS) for the analysis of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) and dioxin-like polychlorinated biphenyls (PCBs) in food and feed. Comprehensive two-dimensional GC–micro electron capture detection (GC×GC-μECD) was tested and all relevant (according to the World Health Organisation, WHO) PCDD/Fs and PCBs could be separated when using a DB-XLB/LC-50 column combination. Validation tests by two laboratories showed that detectability, repeatability, reproducibility and accuracy of GC×GC-μECD are all statistically consistent with GC-HRMS results. A limit of detection of 0.5 pg WHO PCDD/F tetrachlorodibenzo-p-dioxin equivalency concentration per gram of fish oil was established. The reproducibility was less than 10%, which is below the recommended EU value for reference methods (less than 15%). Injections of vegetable oil extracts spiked with PCBs, polychlorinated naphthalenes and diphenyl ethers at concentrations of 200 ng/g showed no significant impact on the dioxin results, confirming in that way the robustness of the method. The use of GC×GC-μECD as a routine method for food and feed analysis is therefore recommended. However, the data evaluation of low dioxin concentrations is still laborious owing to the need for manual integration. This makes the overall analysis costs higher than those of GC-HRMS. Further developments of software are needed (and expected) to reduce the data evaluation time. Combination of the current method with pressurised liquid extraction with in-cell cleanup will result in further reduction of analysis costs.

  • 45.
    Haglund, Peter
    et al.
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Spinnel, Erik
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    A Modular Approach to Pressurized Liquid Extraction with In-Cell Cleanup2010Inngår i: LC GC North America, ISSN 1527-5949, E-ISSN 1939-1889, Vol. 28, nr 7, s. 544-+Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    A new concept for the extraction of solid samples has been developed. The popular pressurized liquid extraction (PLE) technique has been modified so that the extraction cell can be divided, which greatly increases the flexibility and versatility of this technique. The system uses simple adapters to couple commercially available extraction cells, which can be loaded with either sample or adsorbents. These segmented extraction cells make it possible to selectively retain analytes or matrix to achieve simultaneous extraction and cleanup or fractionation. The ultimate aim is to perform simultaneous extraction and cleanup and obtain a purified extract that is ready for instrumental analysis, all in line with current trends in analytical chemistry to automate and streamline the analytical procedures to reduce the analysis costs, solvent consumption, and manual labor, and increase the quality of analysis. Selected modes of operations are presented and a few recent environmental applications of modular PLE are reviewed.

  • 46.
    Haglund, Peter
    et al.
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Spinnel, Erik
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    A Modular Approach to Pressurized Liquid Extraction with In-Cell Cleanup2011Inngår i: LC GC North America, ISSN 1527-5949, E-ISSN 1939-1889, nr Suppl., s. 66-72Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    A new concept for the extraction of solid samples has been developed. The popular pressurized liquid extraction (PLE) technique has been modified so that the extraction cell can be divided, which greatly increases the flexibility and versatility of this technique. The system uses simple adapters to couple commercially available extraction cells, which can be loaded with either sample or adsorbents. These segmented extraction cells make it possible to selectively retain analytes or matrix to achieve simultaneous extraction and cleanup or fractionation. The ultimate aim is to perform simultaneous extraction and cleanup and obtain a purified extract that is ready for instrumental analysis, all in line with current trends in analytical chemistry to automate and streamline the analytical procedures to reduce the analysis costs, solvent consumption, and manual labor, and increase the quality of analysis. Selected modes of operations are presented and a few recent environmental applications of modular PLE are reviewed.

  • 47.
    Haglund, Peter
    et al.
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Wiberg, Karin
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Determination of the gas chromatographic elution sequences of the (+)- and (-)-enantiomers of stable atropistomeric PCBs on Chirasil-Dex1996Inngår i: HRC Journal of High Resolution Chromatography, ISSN 0935-6304, E-ISSN 1521-4168, Vol. 19, nr 7, s. 373-376Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    Pure enantiomers of chiral (atropisomeric) polychlorinated biphenyls (PCBs) obtained by high-performance liquid chromatography were used to establish the gas chromatographic elution sequences of the (+)- and (−)-enantiomers of six PCB atropisomers on Chirasil-Dex. The elution order was found to be (−/+) for PCBs 84, 132, 136, and 176 and (+/−) for PCBs 135 and 174. The retention characteristics of all 19 tri- and tetra-ortho atropisomeric PCBs were also investigated. Nine of the atropisomers could be separated using this chiral selector. PCBs 95, 132, and 149 were completely resovled and PCBs 84, 91, 135, 136, 174, and 176 were partially separated (R = 0.7–0.9). All of the separated congeners are 2,3,6-substituted in at least one ring, and conversely – none of the congeners that lacks 2,3,6-substitution could be separated. Thus, chiral recognition and enantiomer separation seems to be strongly governed by 2,3,6-substitution.

  • 48.
    Harju, Mikael
    et al.
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Bergman, Anders
    Olsson, Mats
    Roos, Anna
    Haglund, Peter
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Determination of atropisomeric and planar polychlorinated biphenyls, their enantiomeric fractions and tissue distribution in grey seals using comprehensive 2D gas chromatography2003Inngår i: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1019, nr 1-2, s. 127-142Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    High prevalence of uterine occlusions and sterility is found among Baltic ringed and grey seal. Polychlorinated biphenyls (CBs) are suspected to be the main cause. The CB concentrations are higher in affected than in healthy animals, but the natural variation is considerable. Thus, it might be possible to assess the health status of seals by CB analysis. The ratios of chiral compounds (enantiomeric fractions (EFs)) such as atropisomeric CBs are of particular interest, since these may reflect differences in metabolic rates. An analytical procedure was developed and used to determine the levels of atropisomeric CBs, planar-CBs (WHO-PCBs) and total CBs in seals of different health status. Comprehensive 2D gas chromatography (GC×GC) was used to separate the target analytes from other CBs and interferences and a micro electron-capture detector (μECD) was used for detection. EFs of the atropisomeric CBs were difficult to determine as the levels were low and the interferences many. Two column combinations had to be used to avoid biased results—both had a chiral column as first-dimension column. The second-dimension column was coated with either a high-polarity cyanopropyl or a liquid crystal phase. EFs were determined for five atropisomeric CBs, i.e. CBs 91, 95, 132, 149 and 174. The results were verified by GC×GC–time-of-flight mass spectrometry (TOF-MS). Some atropisomeric CBs had EFs that deviated strongly from the racemic-mixture value. The deviations were larger in liver than blubber, which indicates enantioselective metabolism. However, there was no selective passage of the studied atropisomeric CBs across placenta and no selective blood–brain barrier. Similarly, no correlation between EFs and health status was observed, although there was a correlation between the total CB levels and health status.

  • 49. Harley, Steven J.
    et al.
    Ohlin, C. Andre
    Casey, William H.
    Geochemical kinetics via the Swift-Connick equations and solution NMR2011Inngår i: Geochimica et Cosmochimica Acta, ISSN 0016-7037, E-ISSN 1872-9533, Vol. 75, nr 13, s. 3711-3725Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    Signal analysis in Nuclear Magnetic Resonance spectroscopy is among the most powerful methods to quantify reaction rates in aqueous solutions. To this end, the Swift-Connick approximations to the Bloch-McConnell equations have been used extensively to estimate rate parameters for elementary reactions. The method is primarily used for O-17 NMR in aqueous solutions, but the list of geochemically relevant nuclei that can be used is long, and includes Si-29, Al-27, F-19, C-13 and many others of particular interest to geochemists. Here we review the derivation of both the Swift-Connick and Bloch-McConnell equations and emphasize assumptions and quirks. For example, the equations were derived for CW-NMR, but are used with modern pulse FT-NMR and can be applied to systems that have exchange rates that are shorter than the lifetime of a typical pulse. The method requires a dilute solution where the minor reacting species contributes a negligible amount of total magnetization. We evaluate the sensitivity of results to this dilute-solution requirement and also highlight the need for chemically well-defined systems if reliable data are to be obtained. The limitations in using longitudinal relaxation to estimate reaction rate parameters are discussed. Finally, we provide examples of the application of the method, including ligand exchanges from aqua ions and hydrolysis complexes, that emphasize its flexibility. Once the basic requirements of the Swift-Connick method are met, it allows geochemists to establish rates of elementary reactions. Reactions at this scale lend themselves well to methods of computational simulation and could provide key tests of accuracy. (C) 2011 Elsevier Ltd. All rights reserved.

  • 50.
    Hemström, Petrus
    et al.
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Nygren, Yvonne
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Björn, Erik
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Irgum, Knut
    Umeå universitet, Teknisk-naturvetenskapliga fakulteten, Kemiska institutionen.
    Alternative organic solvents for HILIC separation of cisplatin species with on-line ICP-MS detection2008Inngår i: Journal of Separation Science, ISSN 1615-9306, E-ISSN 1615-9314, Vol. 31, nr 4, s. 599-603Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    Several low volatile organic solvents were evaluated as organic modifiers in eluents for HILIC separations of cisplatin species to optimize the on-line coupling of HILIC to inductively coupled plasma MS (ICP-MS). The aim was to identify a solvent giving low solvent vapor loading of the ICP, to maximize analyte sensitivity and minimize carbon depositions on instrumental parts, while retaining chromatographic performance. The best overall performance of the HILIC-ICP-MS system for the analysis of cisplatin was achieved using 1,4-dioxane as eluent, yielding high retention and an HILIC type retention mechanism, at the expense of a 50% drop in column efficiency due to the higher viscosity of 1,4-dioxane compared to the more commonly used HILIC solvent ACN. Using 1,4-dioxane as solvent in HILIC provides the best compromise between carbon deposition and separation efficiency among a series of high-boiling water-miscible solvents tested.

1234 1 - 50 of 182
RefereraExporteraLink til resultatlisten
Permanent link
Referera
Referensformat
  • apa
  • ieee
  • modern-language-association-8th-edition
  • vancouver
  • Annet format
Fler format
Språk
  • de-DE
  • en-GB
  • en-US
  • fi-FI
  • nn-NO
  • nn-NB
  • sv-SE
  • Annet språk
Fler språk
Utmatningsformat
  • html
  • text
  • asciidoc
  • rtf