| 1. |
- Bashkanov, M., et al.
(författare)
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Double-Pionic Fusion of Nuclear Systems and the "ABC" Effect : Approaching a Puzzle by Exclusive and Kinematically Complete Measurements
- 2009
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Ingår i: Physical Review Letters. - 0031-9007 .- 1079-7114. ; 102:5, s. 052301-
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Tidskriftsartikel (refereegranskat)abstract
- The ABC effect-a puzzling low-mass enhancement in the pi pi invariant mass spectrum, first observed by Abashian, Booth, and Crowe-is well known from inclusive measurements of two-pion production in nuclear fusion reactions. Here we report on the first exclusive and kinematically complete measurements of the most basic double-pionic fusion reaction pn -> d pi(0)pi(0) at beam energies of 1.03 and 1.35 GeV. The measurements, which have been carried out at CELSIUS-WASA, reveal the ABC effect to be a (pi pi)(I=L=0) channel phenomenon associated with both a resonancelike energy dependence in the integral cross section and the formation of a Delta Delta system in the intermediate state. A corresponding simple s-channel resonance ansatz provides a surprisingly good description of the data.
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| 2. |
- Bargholtz, Chr., et al.
(författare)
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Measurement of the eta -> pi(+)pi(-)e(+)e(-) decay branching ratio
- 2007
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Ingår i: Physics Letters B. - : Elsevier BV. - 0370-2693 .- 1873-2445. ; 644:5-6, s. 299-303
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Tidskriftsartikel (refereegranskat)abstract
- The reaction pd -> He-3 eta at threshold was used to provide a clean source of eta mesons for decay studies with the WASA detector at CELSIUS. The branching ratio of the decay eta -> pi(+)pi(-)e(+)e(-) is measured to be (4.3 +/- 1.3 +/- 0.4) x 10(-4).
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| 3. |
- Bargholtz, Chr., et al.
(författare)
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The WASA detector facility at CELSIUS
- 2008
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Ingår i: Nuclear Instruments and Methods in Physics Research Section A. - : Elsevier BV. - 0168-9002 .- 1872-9576. ; 594:3, s. 339-350
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Tidskriftsartikel (refereegranskat)abstract
- The WASA 4 pi multidetector system, aimed at investigating light meson production in light ion collisions and eta meson rare decays at the CELSIUS storage ring in Uppsala is presented. A unique feature of the system is the use of hydrogen pellets as internal targets for the first time. A detailed description of the design, together with the anticipated and achieved performance parameters are given. (C) 2008 Elsevier B.V. All rights reserved.
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| 4. |
- Schönning, Karin, et al.
(författare)
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Polarisation of the omega meson in the pd -> He-3 omega reaction at 1360 and 1450 MeV
- 2008
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Ingår i: Physics Letters B. - elsevier : Elsevier BV. - 0370-2693 .- 1873-2445. ; 668:4, s. 258-262
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Tidskriftsartikel (refereegranskat)abstract
- The tensor polarisation of omega mesons produced in the pd -> He-3 omega reaction has been studied at two energies near threshold. The 3 He nuclei were detected in coincidence with the pi(0)pi(+)pi(-) or pi(0)gamma decay products of the omega. in contrast to the case of phi-meson production, the omega mesons are found to be unpolarised. This brings into question the applicability of the Okubo-Zweig-lizuka rule when comparing the production of vector mesons in low energy hadronic reactions.
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| 5. |
- Barclay, Victoria K. H., et al.
(författare)
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Acidic transformation of nordiazepam can affect recovery estimate during trace analysis of diazepam and nordiazepam in environmental water samples by liquid chromatography-tandem mass spectrometry
- 2019
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Ingår i: Analytical and Bioanalytical Chemistry. - : SPRINGER HEIDELBERG. - 1618-2642 .- 1618-2650. ; 411:17, s. 3919-3928
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Tidskriftsartikel (refereegranskat)abstract
- In this study, a special interest was focused on the stability of diazepam and nordiazepam in aqueous samples at acidic and neutral pH. The aim of the study was to isolate and illustrate one of the many possible sources of error that can be encountered when developing and validating analytical methods. This can be of particular importance when developing multi-analyte methods where there is limited time to scrutinize the behavior of each analyte. A method was developed for the analysis of the benzodiazepines diazepam and nordiazepam in treated wastewater. The samples were extracted by solid phase extraction, using SPEC C18AR cartridges, and analyzed by the use of liquid chromatography, with a C18 stationary phase, coupled to tandem mass spectrometry. Environmental water samples are often acidified during storage to reduce the microbial degradation of the target compounds and to preserve the sample. In some cases, the samples are acidified before extraction. In this study, it was found that a chemical equilibrium between nordiazepam and a transformation product could cause inaccurately high extraction recovery values when the samples were stored at low sample pH. The stability of nordiazepam was shown to be low at pH3. Within 12days, 20% of the initial concentration of nordiazepam was transformed. Interestingly, the transformed nordiazepam was shown to be regenerated and reformed to nordiazepam during sample handling. At a sample pH of 7, diazepam and nordiazepam were stable for 12days. It was concluded that great care must be taken when acidifying water samples containing nordiazepam during storage or extraction. The storage and the extraction should be conducted at neutral pH if no internal standard is used to compensate for degradation and conversion of nordiazepam. The developed method was validated in treated wastewater and applied for the quantification of diazepam and nordiazepam in treated wastewater samples.
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| 6. |
- Barclay, Victoria K. H., et al.
(författare)
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Trace analysis of fluoxetine and its metabolite norfluoxetine : Part I: Development of a chiral liquid chromatography-tandem mass spectrometry method for wastewater samples
- 2011
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Ingår i: Journal of Chromatography A. - : Elsevier BV. - 0021-9673 .- 1873-3778. ; 1218:33, s. 5587-5596
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Tidskriftsartikel (refereegranskat)abstract
- An enantioselective method for the determination of fluoxetine (a selective serotonin reuptake inhibitor) and its pharmacologically active metabolite norfluoxetine has been developed for raw and treated wastewater samples. The stable isotope-labeled fluoxetine and norfluoxetine were used in an extended way for extraction recovery calculations at trace level concentrations in wastewater. Wastewater samples were enriched by solid phase extraction (SPE) with Evolute CX-50 extraction cartridges. The obtained extraction recoveries ranged between 65 and 82% in raw and treated wastewater at a trace level concentration of 50 pM (15-16 ng L(-1)). The target compounds were identified by the use of chiral liquid chromatography tandem mass spectrometry (LC-MS/MS) in selected reaction monitoring (SRM) mode. The enantiomers were successfully resolved on a chiral alpha(1)-acid glycoprotein column (chiral AGP) with acetonitrile and 10 mM ammonium acetate buffer at pH 4.4 (3/97, v/v) as the mobile phase. The effects of pH, amount of organic modifier and buffer concentration in the mobile phase were investigated on the enantiomeric resolution (R(s)) of the target compounds. Enantiomeric R(s)-values above 2.0 (1.03 RSD%, n = 3) were achieved for the enantiomers of fluoxetine and norfluoxetine in all mobile phases investigated. The method was validated by assessing parameters such as cross-contamination and carryover during SPE and during LC analysis. Cross-talk effects were examined during the detection of the analytes in SRM mode. In addition, the isotopic purity of fluoxetine-d(5) and norfluoxetine-d(5) were assessed to exclude the possibility of self-contamination. The interassay precision of the chromatographic separation was excellent, with relative standard deviations (RSD) equal to or lower than 0.56 and 0.81% in raw and treated wastewaters, respectively. The method detection and quantification limits (respectively, MDL and MQL) were determined by the use of fluoxetine-d5 and norfluoxetine-d5. The MQL for the single enantiomers ranged from 12 to 14 pM (3.6-4.3 ng L(-1)) in raw wastewater and from 3 to 4 pM (0.9-1 ng L(-1)) in treated wastewater. The developed method has been employed for the quantification of (R)-fluoxetine, (S)-fluoxetine and the enantiomers of norfluoxetine in raw and treated wastewater samples to be presented in Part II of this study.
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| 7. |
- Barclay, Victoria K H, et al.
(författare)
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Trace analysis of fluoxetine and its metabolite norfluoxetine. Part II : Enantioselective quantification and studies of matrix effects in raw and treated wastewater by solid phase extraction and liquid chromatography-tandem mass spectrometry
- 2012
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Ingår i: Journal of Chromatography A. - : Elsevier BV. - 0021-9673 .- 1873-3778. ; 1227, s. 105-114
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Tidskriftsartikel (refereegranskat)abstract
- The isotope-labeled compounds fluoxetine-d5 and norfluoxetine-d5 were used to study matrix effects caused by co-eluting compounds originating from raw and treated wastewater samples, collected in Uppsala, Sweden. The matrix effects were investigated by the determination of matrix factors (MF) and by a post-column infusion method. The matrix factors were determined to be 38–47% and 71–86% for the enantiomers of norfluoxetine-d5 and fluoxetine-d5, respectively. The influence of matrix effects when quantifying the enantiomers of the active pharmaceutical ingredient and the metabolite in wastewater samples with LC–MS/MS is discussed and methods to overcome the problem are presented. The enantiomeric concentrations of fluoxetine and its human metabolite norfluoxetine, quantified by a one-point calibration method, were 12–52 pM (3.5–16 ng L−1) in raw wastewater and 4–48 pM (1.2–15 ng L−1) in treated wastewater. Furthermore, the calculated enantiomeric fractions (EF) of the substances were found to be between 0.68 and 0.71 in both matrices. Neither the EF values for fluoxetine nor those for norfluoxetine were significantly different in the raw wastewater compared to the treated wastewater. Interestingly, the concentration of (S)-fluoxetine was found to be higher than the concentration of (R)-fluoxetine in both raw and treated wastewater. These results are different from other results presented in the literature, which shows that the relative concentrations of the enantiomers of a chiral active pharmaceutical ingredient might be significantly different in wastewater samples from different treatment systems. We report, for the first time, the concentrations of the enantiomers of norfluoxetine in wastewater samples. The concentrations of (S)-norfluoxetine were found to be higher than the concentration of (R)-norfluoxetine in the raw as well as in the treated wastewater samples.
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| 8. |
- Bashkanov, M., et al.
(författare)
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Measurement of the slope parameter for the η → 3π0 decay in the pp → ppη reaction
- 2007
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Ingår i: Physical Review C. Nuclear Physics. - 0556-2813 .- 1089-490X. ; 76:4, s. 048201-
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Tidskriftsartikel (refereegranskat)abstract
- The CELSIUS-WASA setup is used to measure the 3π0 decay of η mesons produced in pp interactions with beam kinetic energies of 1.36 and 1.45 GeV. The efficiency-corrected Dalitz plot and density distributions for this decay are shown, together with a fit of the quadratic slope parameter α yielding α = −0.026 ± 0.010(stat) ± 0.010(syst). This value is compared to recent experimental results and theoretical predictions.
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| 9. |
- Berlowski, M., et al.
(författare)
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Measurement of eta meson decays into lepton-antilepton pairs
- 2008
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Ingår i: Physical Review D. Particles and fields. - : American Physical Society. - 0556-2821 .- 1089-4918. ; 77:3, s. 032004-
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Tidskriftsartikel (refereegranskat)abstract
- A search for rare lepton decays of the eta meson was performed using the WASA detector at CELSIUS. Two candidates for double Dalitz decay eta -> e(+)e(-)e(+)e(-) events are reported with a background of 1.3 +/- 0.2 events. This allows to set an upper limit to the branching ratio of 9.7x10(-5) (90% CL). The branching ratio for the decay eta -> e(+)e(-)gamma is determined to (7.8 +/- 0.5(stat)+/- 0.8(syst))x10(-3) in agreement with world average value. An upper limit (90% CL) for the branching ratio for the eta -> e(+)e(-) decay is 2.7x10(-5) and a limit for the sum of the eta ->mu(+)mu(-)mu(+)mu(-) and eta ->pi(+)pi(-)mu(+)mu(-) decays is 3.6x10(-4).
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| 10. |
- Fransson, Anette E, et al.
(författare)
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Hydrogen Inhalation Protects against Ototoxicity Induced by Intravenous Cisplatin in the Guinea Pig
- 2017
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Ingår i: Frontiers in Cellular Neuroscience. - : Frontiers Media SA. - 1662-5102. ; 11
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Tidskriftsartikel (refereegranskat)abstract
- Introduction: Permanent hearing loss and tinnitus as side-effects from treatment with the anticancer drug cisplatin is a clinical problem. Ototoxicity may be reduced by co-administration of an otoprotective agent, but the results in humans have so far been modest.Aim: The present preclinical in vivo study aimed to explore the protective efficacy of hydrogen (H2) inhalation on ototoxicity induced by intravenous cisplatin.Materials and Methods: Albino guinea pigs were divided into four groups. The Cispt (n = 11) and Cispt+H2 (n = 11) groups were given intravenous cisplatin (8 mg/kg b.w., injection rate 0.2 ml/min). Immediately after, the Cispt+H2 group also received gaseous H2 (2% in air, 60 min). The H2 group (n = 5) received only H2 and the Control group (n = 7) received neither cisplatin nor H2. Ototoxicity was assessed by measuring frequency specific ABR thresholds before and 96 h after treatment, loss of inner (IHCs) and outer (OHCs) hair cells, and by performing densitometry-based immunohistochemistry analysis of cochlear synaptophysin, organic transporter 2 (OCT2), and copper transporter 1 (CTR1) at 12 and 7 mm from the round window. By utilizing metabolomics analysis of perilymph the change of metabolites in the perilymph was assessed.Results: Cisplatin induced electrophysiological threshold shifts, hair cell loss, and reduced synaptophysin immunoreactivity in the synapse area around the IHCs and OHCs. H2 inhalation mitigated all these effects. Cisplatin also reduced the OCT2 intensity in the inner and outer pillar cells and in the stria vascularis as well as the CTR1 intensity in the synapse area around the IHCs, the Deiters' cells, and the stria vascularis. H2 prevented the majority of these effects.Conclusion: H2 inhalation can reduce cisplatin-induced ototoxicity on functional, cellular, and subcellular levels. It is proposed that synaptopathy may serve as a marker for cisplatin ototoxicity. The effect of H2 on the antineoplastic activity of cisplatin needs to be further explored.
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| 11. |
- Haglind, Alfred, 1986-, et al.
(författare)
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Major signal suppression from metal ion clusters in SFC/ESI-MS : Cause and Effects
- 2018
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Ingår i: Journal of chromatography. B. - : Elsevier BV. - 1570-0232 .- 1873-376X. ; 1084, s. 96-105
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Tidskriftsartikel (refereegranskat)abstract
- The widening application area of SFC-MS with polar analytes and water-containing samples facilitates the use of quick and simple sample preparation techniques such as “dilute and shoot” and protein precipitation. This has also introduced new polar interfering components such as alkali metal ions naturally abundant in e.g. blood plasma and urine, which have shown to be retained using screening conditions in SFC/ESI-TOF-MS and causing areas of major ion suppression. Analytes co-eluting with these clusters will have a decreased signal intensity, which might have a major effect on both quantification and identification. When investigating the composition of the alkali metal clusters using accurate mass and isotopic pattern, it could be concluded that they were previously not described in the literature. Using NaCl and KCl standards and different chromatographic conditions, varying e.g. column and modifier, the clusters proved to be formed from the alkali metal ions in combination with the alcohol modifier and make-up solvent. Their compositions were [(XOCH3)n+X]+, [(XOH)n+X]+, [(X2CO3)n+X]+ and [(XOOCOCH3)n+X]+ for X= Na+ or K+ in ESI+. In ESI-, the clusters depended more on modifier, with [(XCl)n+Cl]- and [(XOCH3)n+OCH3]- mainly formed in pure methanol and [(XOOCH)n+OOCH]- when 20 mM NH4Fa was added.To prevent the formation of the clusters by avoiding methanol as modifier might be difficult, as this is a widely used modifier providing good solubility when analyzing polar compounds in SFC. A sample preparation with e.g. LLE would remove the alkali ions, however also introducing a time consuming and discriminating step into the method. Since the alkali metal ions were retained and affected by chromatographic adjustments as e.g. mobile phase modifications, a way to avoid them could therefore be chromatographic tuning, when analyzing samples containing them.
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| 12. |
- Pauly, C., et al.
(författare)
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The pp→ppπππ reaction channels in the threshold region
- 2007
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Ingår i: Physics Letters B. - : Elsevier BV. - 0370-2693 .- 1873-2445. ; 649:2-3, s. 122-127
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Tidskriftsartikel (refereegranskat)abstract
- The cross section for direct neutral and charged three pion production in pp interactions was measured at excess energies in the range 160–216 MeV. That comprises the first measurement of the pp→ppπ0π0π0 reaction and the direct comparison with the pp→ppπ+π−π0 process. The experiment was performed above the η meson production threshold and the cross section could be directly normalized to the cross section of the pp→ppη reaction, with the η decaying into 3 pions. Since the same final states are selected, the measurement has a low systematical error. The measured cross section ratio σ(pp→ppπ+π−π0)/σ(pp→ppπ0π0π0) is compared to predictions of dominance of different isobars in the intermediate state.
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| 13. |
- Pettersson, Henrik, et al.
(författare)
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eta PRODUCTION IN PROTON-PROTON COLLISIONS AT 72 MeV EXCESS ENERGY
- 2009
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Ingår i: International Journal of Modern Physics A. - 0217-751X .- 1793-656X. ; 24:2-3, s. 446-449
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Tidskriftsartikel (refereegranskat)abstract
- The production of eta mesons at an excess energy of 72 MeV has been studied in the reaction pp -> pp(eta)gamma gamma. It is shown that a simple model with Pp. final states included reproduces observed differential distributions better than the same model restricted to Ss, Sd and Ds final states. The strong influence of the Pp states could be taken as an indication of rho dominance within an one boson exchange model for the excitation of N*(1535).
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| 14. |
- Pierre, Pernilla Videhult, et al.
(författare)
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Cisplatin-induced metabolome changes in serum : an experimental approach to identify markers for ototoxicity
- 2017
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Ingår i: Acta Oto-Laryngologica. - : Informa UK Limited. - 0001-6489 .- 1651-2251. ; 137:10, s. 1024-1030
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Tidskriftsartikel (refereegranskat)abstract
- BACKGROUND: Ototoxicity from treatment with the anticancer drug cisplatin remains a clinical problem. A wide range of intracellular targets of cisplatin has been found in vivo.AIM: To investigate cisplatin-induced change of the serum metabolite profile and its association with ototoxicity.MATERIAL AND METHODS: Guinea pigs (n = 14) were treated with cisplatin (8 mg/kg b.w., i.v.) 30 min after administration of the otoprotector candidate sodium thiosulfate (group STS; n = 7) or sodium chloride (group NaCl; n = 7). Ototoxicity was evaluated by ABR (3-30 kHz) before and 4 d after drug treatment, and by assessment of hair cell loss. A blood sample was drawn before and 4 d after drug treatment and the polar metabolome in serum was analyzed using LC-MS.RESULTS: Cisplatin-treatment caused significant threshold elevations and outer hair cell (OHC) loss in both groups. The ototoxicity was generally lower in group STS, but a significant difference was reached only at 30 kHz (p = .007). Cisplatin treatment altered the metabolite profile significantly and similarly in both groups. A significant inverse correlation was found between L-acetylcarnitine, N-acetylneuraminic acid, ceramide, and cysteinylserine and high frequency hearing loss in group NaCl. The implication of these correlations should be explored in targeted studies.
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| 15. |
- Steffen, Karin, 1989-, et al.
(författare)
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Oceanographic setting influences the prokaryotic community and metabolome in deep-sea sponges
- 2022
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Ingår i: Scientific Reports. - : NATURE RESEARCH. - 2045-2322. ; 12
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Tidskriftsartikel (refereegranskat)abstract
- Marine sponges (phylum Porifera) are leading organisms for the discovery of bioactive compounds from nature. Their often rich and species-specific microbiota is hypothesised to be producing many of these compounds. Yet, environmental influences on the sponge-associated microbiota and bioactive compound production remain elusive. Here, we investigated the changes of microbiota and metabolomes in sponges along a depth range of 1232 m. Using 16S rRNA gene amplicon sequencing and untargeted metabolomics, we assessed prokaryotic and chemical diversities in three deep-sea sponge species: Geodia barretti, Stryphnus fortis, and Weberella bursa. Both prokaryotic communities and metabolome varied significantly with depth, which we hypothesized to be the effect of different water masses. Up to 35.5 % of microbial ASVs (amplicon sequence variants) showed significant changes with depth while phylum-level composition of host microbiome remained unchanged. The metabolome varied with depth, with relative quantities of known bioactive compounds increasing or decreasing strongly. Other metabolites varying with depth were compatible solutes regulating osmolarity of the cells. Correlations between prokaryotic community and the bioactive compounds in G. barretti suggested members of Acidobacteria, Proteobacteria, Chloroflexi, or an unclassified prokaryote as potential producers.
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| 16. |
- Stenholm, Åke, et al.
(författare)
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Removal of diclofenac from a non-sterile aqueous system using Trametes versicolor with an emphasis on adsorption and biodegradation mechanisms
- 2019
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Ingår i: Environmental technology. - : Informa UK Limited. - 0959-3330 .- 1479-487X. ; 40:19, s. 2460-2472
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Tidskriftsartikel (refereegranskat)abstract
- This paper describes the search for procedures through which the xenobiotic pollutant diclofenac can be removed from non-sterile aquatic systems. Specifically, adsorption to solid supports (carriers) in combination with biodegradation by non-immobilized and immobilized white rot fungus Trametes versicolor were investigated. Batch experiments using polyurethane foam (PUF)-carriers resulted in 99.9% diclofenac removal after 4 h, with monolayer adsorption of diclofenac to carrier and glass surfaces accounting for most of the diclofenac decrease. Enzymatic reactions contributed less, accounting for approximately < 0.5% of this decrease. In bioreactor experiments using PUF-carriers, an initial 100% removal was achieved with biodegradation contributing approximately 7%. In batch experiments that utilized polyethylene-carriers with negligible immobilization of Trametes versicolor, a 98% total diclofenac removal was achieved after one week, with a biodegradation contribution of approximately 14%. Five novel enzyme-catalyzed biodegradation products were tentatively identified in the batch-wise and bioreactor experiments using full scan ultra-high-performance liquid chromatography-quadrupole/time of flight mass spectrometry. Both reduction and oxidation products were found, with the contents estimated to be at µg L-1 concentration levels.
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| 17. |
- Stenholm, Åke, et al.
(författare)
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Removal of nonylphenol polyethoxylates by adsorption on polyurethane foam and biodegradation using immobilized Trametes versicolor
- 2020
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Ingår i: Science of the Total Environment. - : Elsevier BV. - 0048-9697 .- 1879-1026. ; 724
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Tidskriftsartikel (refereegranskat)abstract
- Nonylphenol polyethoxylates (NPEOs) are banned in EU due to their endocrine disrupting properties. In a proof of concept study including continuous reactor lab-scale experiments, polyurethane foam (PUF)-immobilized Trametes versicolor was used to reduce the concentration levels of these compounds in an acidic nutrient solution over an 18-day period. Biodegradation and adsorption were identified as the major removal principles. A 90% removal was achieved by solely biodegradation in an experimental setup in which steady state conditions occurred, including NPEO-saturated glass and PUF surfaces. Biotransformation products containing mono- and di-ethoxylated nonylphenol, nonylphenol (NP1EO, NP2EO, NP) and nonylphenol polyethoxy carboxylates (NPECs) were tentatively identified.The maximum static NPEO adsorption capacity of PUF (determined with Erlenmeyer flask experiment) was calculated to 106 mg g−1, and the adsorption was described by the Langmuir isotherm equation. The corresponding maximum dynamic adsorption capacity (determined by continuous reactor experiment) was 100 mg g−1. These findings show that PUF is an excellent adsorbent to NPEOs. Therefore, PUF can either be used as a stand-alone adsorbent to NPEOs or as an immobilizing agent for Trametes versicolor through which a highly efficient biodegradation of these potentially harmful compounds can be achieved. The findings can be of importance in the search for alternative methods to remove NPEOs in process effluents.
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| 18. |
- Svan, Alfred, et al.
(författare)
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Identification of transformation products from -blocking agents formed in wetland microcosms using LC-Q-ToF
- 2016
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Ingår i: Journal of Mass Spectrometry. - : Wiley. - 1076-5174 .- 1096-9888. ; 51:3, s. 207-218
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Tidskriftsartikel (refereegranskat)abstract
- Identification of degradation products from trace organic compounds, which may retain the biological activity of the parent compound, is an important step in understanding the long-term effects of these compounds on the environment. Constructed wetlands have been successfully utilized to remove contaminants from wastewater effluent, including pharmacologically active compounds. However, relatively little is known about the transformation products formed during wetland treatment. In this study, three different wetland microcosm treatments were used to determine the biotransformation products of the -adrenoreceptor antagonists atenolol, metoprolol and propranolol. LC/ESI-Q-ToF run in the MSE and MS/MS modes was used to identify and characterize the degradation products through the accurate masses of precursor and product ions. The results were compared with those of a reference standard when available. Several compounds not previously described as biotransformation products produced in wetlands were identified, including propranolol-O-sulfate, 1-naphthol and the human metabolite N-deaminated metoprolol. Transformation pathways were significantly affected by microcosm conditions and differed between compounds, despite the compounds' structural similarities. Altogether, a diverse range of transformation products in wetland microcosms were identified and elucidated using high resolving MS. This work shows that transformation products are not always easily predicted, nor formed via the same pathways even for structurally similar compounds.
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| 19. |
- Svan, Alfred, et al.
(författare)
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Rapid chiral separation of atenolol, metoprolol, propranolol and the zwitterionic metoprolol acid using supercritical fluid chromatography-tandem mass spectrometry - Application to wetland microcosms
- 2015
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Ingår i: Journal of Chromatography A. - : Elsevier BV. - 0021-9673 .- 1873-3778. ; 1409, s. 251-258
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Tidskriftsartikel (refereegranskat)abstract
- A method for enantiomeric separation of the three beta-blocking agents atenolol, metoprolol, propranolol and the zwitterionic metoprolol acid, a major metabolite of both metoprolol and in environmental matrices also atenolol, has been developed. By use of supercritical fluid chromatography and the polysaccharide-based Chiralpak (R) IB-3, all four compounds were simultaneously enantiomerically separated (R-s >1.5) within 8 min. Detection was performed using tandem mass spectrometry, and to avoid isobaric interference between the co-eluting metoprolol and metoprolol acid, the achiral column Acquity (R) UPC2 BEH 2-EP was attached ahead of to the chiral column. Carbon dioxide with 18% methanol containing 0.5% (v/v) of the additives trifluoroacetic acid and ammonia in a 2:1 molar ratio were used as mobile phase. A post column make-up flow (0.3 mL/min) of methanol containing 0.1% (v/v) formic acid was used to enhance the positive electrospray ionization. Detection was carried out using a triple quadrupole mass spectrometer operating in the selected reaction monitoring mode, using one transition per analyte and internal standard. The method was successfully applied for monitoring the enantiomeric fraction change over time in a laboratory scale wetland degradation study. It showed good precision, recovery, sensitivity and low effect of the sample matrix.
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| 20. |
- Sänger-van de Griend, Cari E, Dr, et al.
(författare)
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Capillary Electrophoresis : an Attractive Technique for Chiral Separations
- 2013
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Ingår i: Chromatography Today. - 1752-8070. ; 6:2, s. 32-37
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Forskningsöversikt (refereegranskat)abstract
- Capillary Electrophoresis (CE) separates compounds that differ in charge to hydrodynamic size ratio and is an excellent technique for the analysis of polar compounds. The technique is particularly applicable to chiral separations. Chiral CE separation is achieved by adding a chiral selector to the so called background electrolyte. The enantiomers then form fast, reversible equilibria with the selector. In this paper a simple method development strategy for basic, acidic and neutral compounds is presented and illustrated with examples and common pitfalls. Some important good working practices (background electrolyte buffer recipes, temperature, corrected peak area, injection, polyimide coating removal from capillary ends) are highlighted, so that a good chiral separation can be developed into a robust analytical method.
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