| 1. |
- Bengtsson, Jörgen, et al.
(författare)
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On-line desalting and determination of morphine, morphine-3-glucuronide and morphine-6-glucuronide in microdialysis and plasma samples using column switching and liquid chromatography/tandem mass spectrometry
- 2005
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Ingår i: Rapid Communications in Mass Spectrometry. - : John Wiley & Sons. - 0951-4198 .- 1097-0231. ; 19:15, s. 2116-2122
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Tidskriftsartikel (refereegranskat)abstract
- A sensitive and reproducible method for the determination of morphine and the metabolites morphine-3-glucuronide (M3G) and morphine-6-glucuronide (M6G) was developed. The method was validated for perfusion fluid used in microdialysis as well as for sheep and human plasma. A C18 guard column was used to desalt the samples before analytical separation on a ZIC HILIC (hydrophilic interaction chromatography) column and detection with tandem mass spectrometry (MS/MS). The mobile phases were 0.05% trifluoroacetic acid (TFA) for desalting and acetonitrile/5 mM ammonium acetate (70:30) for separation. Microdialysis samples (5 microL) were directly injected onto the system. The lower limits of quantification (LLOQ) for morphine, M3G and M6G were 0.50, 0.22 and 0.55 ng/mL, respectively, and the method was linear from LLOQ to 200 ng/mL. For plasma, a volume of 100 microL was precipitated with acetonitrile containing internal standards (deuterated morphine and metabolites). The supernatant was evaporated and reconstituted in 0.05% TFA before the desalting process. The LLOQs for sheep plasma were 2.0 and 3.1 ng/mL and the ranges were 2.0-2000 and 3.1-3100 ng/mL for morphine and M3G, respectively. For human plasma, the LLOQs were 0.78, 1.49 and 0.53 ng/mL and the ranges were 0.78-500, 1.49-1000 and 0.53-500 ng/mL for morphine, M3G and M6G, respectively.
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| 2. |
- Benkestock, Kurt, et al.
(författare)
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Electrospray ionization mass spectrometry as a tool for determination of drug binding sites to human serum albumin by noncovalent interaction
- 2005
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Ingår i: Rapid Communications in Mass Spectrometry. - : Wiley. - 0951-4198 .- 1097-0231. ; 19:12, s. 1637-1643
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Tidskriftsartikel (refereegranskat)abstract
- Most proteins in blood plasma bind ligands. Human serum albumin (HSA) is the main transport protein with a very high capacity for binding of endogenous and exogenous compounds in plasma. Many pharmacokinetic properties of a drug depend on the level of binding to plasma proteins. This work reports studies of noncovalent interactions by means of nanoelectrospray ionization mass spectrometry (nanoESI-MS) for determination of the specific binding of selected drug candidates to HSA. Warfarin, iopanoic acid and digitoxin were chosen as site-specific probes that bind to the main sites of HSA. Two drug candidates and two known binders to HSA were analyzed using a competitive approach. The drugs were incubated with the target protein followed by addition of site-specific probes, one at a time. The drug candidates showed predominant affinity to site I (warfarin site). Naproxen and glyburide showed affinity to both sites I and II. The advantages of nanoE-SI-MS for these studies are the sensitivity, the absence of labeled molecules and the short method development time.
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| 3. |
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| 4. |
- Burman, Johan, 1966, et al.
(författare)
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A simplified method of preparing phosphoric acid for stable isotope analyses of carbonates
- 2005
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Ingår i: Rapid Communications in Mass Spectrometry. - : Wiley. - 0951-4198 .- 1097-0231. ; 19:21, s. 3086-3088
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Tidskriftsartikel (refereegranskat)abstract
- In order to produce CO2 for stable isotope analyses (delta(18)O and delta(13)C), carbonate samples are commonly digested in phosphoric acid. The acid recipe here presented is based on phase shifting crystalline orthophosphoric acid of pro-analysis quality to a liquid state through heating, followed by pre-vacuum treatment during a start-up procedure before mass analyses for common acid bath preparation, or adding a small amount of phosphoric pentoxide for single drop equipments, respectively. This methodology results in a final acid concentration of 104%. Copyright (C) 2005 John Wiley & Sons, Ltd.
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| 5. |
- Conrotto, Paolo, et al.
(författare)
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Lys Tag : an easy and robust chemical modification for improved de novo sequencing with a matrix-assisted laser desorption/ionization tandem time-of-flight mass spectrometer
- 2008
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Ingår i: Rapid Communications in Mass Spectrometry. - : Wiley. - 0951-4198 .- 1097-0231. ; 22:12, s. 1823-33
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Tidskriftsartikel (refereegranskat)abstract
- Mass spectrometry using a matrix-assisted laser desorption/ionization (MALDI) time-of-flight (TOF) instrument is a widespread technique for various types of proteomic analysis. Along with an expanding interest in proteomics, there is a strong requirement for the identification of proteins with high confidence from biological samples. Peptide modification by a wide variety of post-translational modifications (PTMs), the existence of different protein isoforms and the presence of uncharacterized genomes of many species, make protein identification through peptide mass fingerprinting (PMF) often unachievable. Peptide de novo sequencing has been proven to be a useful approach to overcome these variables, and efficient derivatization processes are important tools to achieve this goal. In the present work we describe the methodology and experimental applications of a fast, efficient and cheap lysine derivatization. This chemical modification improves the signals from lysine-terminated peptides and can be efficiently used as a lysine-blocking agent in combination with other derivatization techniques. Most importantly, upon peptide fragmentation it generates a neat series of predominantly y-ions, allowing the determination of unambiguous amino acid sequences. Moreover, this chemical compound was used with target-eluted samples, enabling a second, alternative analysis of the same sample in the MALDI mass spectrometer.
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| 6. |
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| 7. |
- Ek, Patrik, et al.
(författare)
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Electrospray Ionization from a Gap with Adjustable Width
- 2006
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Ingår i: Rapid Communications in Mass Spectrometry. - : Wiley. - 0951-4198 .- 1097-0231. ; 20:21, s. 3176-3182
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Tidskriftsartikel (refereegranskat)abstract
- In this paper, we present a new concept for electrospray ionization mass spectrometry, where the sample is applied in a gap which is formed between the edges of two triangular-shaped tips. The size of the spray orifice can be changed by varying the gap width. The tips were fabricated from polyethylene terephthalate film with a thickness of 36 μm. To improve the wetting of the gap and sample confinement, the edges of the tips forming the gap were hydrophilized by means of silicon dioxide deposition. Electrospray was performed with gap widths between 1 and 36 μm and flow rates down to 75 nL/min. The gap width could be adjusted in situ during the mass spectrometry experiments and nozzle clogging could be managed by simply widening the gap. Using angiotensin I as analyte, the signal-to-noise ratio increased as the gap width was decreased, and a shift towards higher charge states was observed. The detection limit for angiotensin I was in the low nM range.
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| 8. |
- Enebro, Jonas, et al.
(författare)
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Improved matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry of carboxymethyl cellulose
- 2006
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Ingår i: Rapid Communications in Mass Spectrometry. - : Wiley. - 0951-4198 .- 1097-0231. ; 20:24, s. 3693-3698
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Tidskriftsartikel (refereegranskat)abstract
- A refined sample preparation procedure for matrix-assisted laser desorption/ionisation time-of-flight mass spectrometry (MALDI-TOFMS) was developed for the evaluation of the degree of substitution (DS) in partially depolymerised carboxymethyl cellulose (CMC). By adding ammonium sulphate to the sample mixture prior to the analysis, good quality mass spectra could be acquired. The usual time-consuming search for 'sweet-spots' at the crystalline rim of the MALDI target spot was also avoided. This quality improvement made it possible to investigate whether various positions on the target spot generated mass spectra in which the measured DS varied. The accuracy and reproducibility of the sample preparation procedure were tested by applying it on three commercial CMCs. The study shows that the DS values that were calculated from the spectra acquired from the centre region of the MALDI target spot were in better agreement with the DS provided by the supplier than were the values obtained from the large crystals at the target spot rim. This observation could be one reasonable explanation for the higher DS values reported in other publications. By applying our refined MALDI sample preparation procedure DS values that were in good agreement with the values provided by the manufacturer could be obtained. This indicates that MALDI-TOFMS of partially depolyrnerised CMCs can be used for an estimation of the DS as a complement to the more established methods, e.g. NMR, titrimetry, and chromatographic techniques.
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| 9. |
- Eriksson, Cecilia, et al.
(författare)
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Time-of-flight secondary ion mass spectrometric analysis of the interface between bone and titanium implants.
- 2008
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Ingår i: Rapid communications in mass spectrometry : RCM. - : Wiley. - 0951-4198 .- 1097-0231. ; 22:7, s. 943-9
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Tidskriftsartikel (refereegranskat)abstract
- Implant healing into bone tissue is a process where the mature bone grows towards and eventually fuses with the implant. In this study we investigated implant healing during 4 weeks with focus on the implant-tissue interface. Our main interest was to study the mineralization process around the implant. Titanium discs were implanted in rat tibia for 2 and 4 weeks. After implantation cross sections of bone and implant were made using a low-speed saw equipped with a diamond wafering blade. One section from each sample was stained with basic fuchsin and micrographed by light microscopy (LM). The other section was analyzed with imaging time-of-flight secondary ion mass spectrometry (TOF-SIMS) using a Bi(3)(+) cluster ion source. This ion source has recently been shown to enable identification of high-mass hydroxyapatite (HA) fragment ions (m/z 291-653) in bone samples. The LM images were used to identify areas suitable for TOF-SIMS analysis. Three areas were selected for mass spectral analysis, corresponding to interface region, bone and soft tissue, from which positive ion spectra were recorded. In the areas identified as bone, high-mass HA fragments ions were found after both 2 and 4 weeks. In the soft tissue area, no high-mass ions were found after 4 weeks. However, after 2 weeks HA-related ions were identified in mineralized spots in areas defined as soft tissue. After 4 but not after 2 weeks, high-mass HA fragment ions were found in the interface region. In conclusion, differences were observed regarding mineralization between 2 and 4 weeks of implantation and between different regions surrounding the implants. Imaging TOF-SIMS analysis using a Bi(3)(+) cluster as ion source enables identification of high-mass HA fragment ions at implant-tissue interfaces in bone. This technique might therefore be useful for biocompatibility assessment and for studying the mineralization process at implant surfaces.
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| 10. |
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| 11. |
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| 12. |
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| 13. |
- Green, Henrik, et al.
(författare)
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Measurement of paclitaxel and its metabolites in human plasma using liquid chromatography/ion trap mass spectrometry with a sonic spray ionization interface
- 2006
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Ingår i: Rapid Communications in Mass Spectrometry. - : Wiley. - 1097-0231 .- 0951-4198. ; 20:14, s. 2183-2189
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Tidskriftsartikel (refereegranskat)abstract
- A quantitative liquid chromatography/ion trap mass spectrometry method for the simultaneous determination of paclitaxel, 6α-hydroxypaclitaxel and p-3'-hydroxypaclitaxel in human plasma has been developed and validated. 6α-,p-3'-Dihydroxypaclitaxel was also quantified using paclitaxel as a reference and docetaxel as an internal standard. The substances were extracted from 0.500 mL plasma using solid-phase extraction. The elution was performed with acetonitrile and the samples were reconstituted in the mobile phase. Isocratic high-performance liquid chromatography analysis was performed by injecting 50 µL of reconstituted material onto a 100 × 3.00 mm C12 column with a methanol:1% trifluoroacetic acid/ammonium trifluoroacetate in H2O 70:30 mobile phase at 350 µL/min. The [M+H]+ ions generated in the sonic spray ionization interface were isolated and fragmented using two serial mass spectrometric methods: one for paclitaxel (transition 854 → 569 & 551) and the dihydroxymetabolite (transition 886 → 585 & 567) and one for the hydroxy metabolites (transition 870 → 585 & 567; transition 870 → 569 & 551) and docetaxel ([M+Na]+, transition 830 → 550). Calibration curves were created ranging between 0.5 and 7500 ng/mL for paclitaxel, 0.5 and 750 ng/mL for 6α-hydroxypaclitaxel, and 0.5 and 400 ng/mL for p-3'-hydroxypaclitaxel. Adduct ion formation was noted and investigated during method development and controlled by mobile phase optimization. In conclusion, a sensitive method for simultaneous quantification of paclitaxel and its metabolites suitable for analysis in clinical studies was obtained.
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| 14. |
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| 15. |
- Gupta, Anubha, et al.
(författare)
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Quantitative determination of cetirizine enantiomers in guinea pig plasma, brain tissue and microdialysis samples using liquid chromatography/tandem mass spectrometry
- 2005
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Ingår i: Rapid Communications in Mass Spectrometry. - : Wiley. - 0951-4198 .- 1097-0231. ; 19:12, s. 1749-1757
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Tidskriftsartikel (refereegranskat)abstract
- Sensitive enantioselective liquid chromatographic assays using tandem mass spectrometric detection were developed and validated for the determination of S-cetirizine (S-CZE) and R-cetirizine (R-CZE) in guinea pig plasma, brain tissue, and microdialysis samples. Enantioselective separation was achieved on an alpha1-acid glycoprotein column within 14 min for all methods. A cetirizine analog, ucb 20028, was used as internal standard. Cetirizine and the internal standard were detected by multiple reaction monitoring using transitions m/z 389.1 --> 200.9 and 396.1 --> 276.1, respectively. The samples were prepared using protein precipitation with acetonitrile. For guinea pig plasma, the assay was linear over the range 0.25-5000 ng/mL for both S-CZE and R-CZE, with a lower limit of quantification (LLOQ) of 0.25 ng/mL. For the brain tissue and microdialysis samples, the assays were linear over the range 2.5-250 ng/g and 0.25-50 ng/mL, respectively, and the LLOQ values were 2.5 ng/g and 0.25 ng/mL, respectively. The intra- and inter-day precision values were < or =7.1% and < or =12.6%, respectively, and the intra- and inter-day accuracy varied by less than +/-8.0% and +/-6.0% of the nominal value, respectively, for both enantiomers in all the matrices investigated.
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| 16. |
- Göttlicher, Sabine
(författare)
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Preparation of starch and soluble sugars of plant material for the analysis of carbon isotope composition: a comparison of methods
- 2009
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Ingår i: Rapid Communications in Mass Spectrometry. - : Wiley. - 0951-4198 .- 1097-0231. ; 23, s. 2476-2488
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Tidskriftsartikel (refereegranskat)abstract
- Starch and soluble sugars are the major photosynthetic products, and their carbon isotope signatures reflect external versus internal limitations of CO(2) fixation. There has been recent renewed interest in the isotope composition of carbohydrates, mainly for use in CO(2) flux partitioning studies at the ecosystem level. The major obstacle to the use of carbohydrates in such studies has been the lack of an acknowledged method to isolate starch and soluble sugars for isotopic measurements. We here report on the comparison and evaluation of existing methods (acid and enzymatic hydrolysis for starch; ion-exchange purification and compound-specific analysis for sugars). The selectivity and reproducibility of the methods were tested using three approaches: (i) an artificial leaf composed of a mixture of isotopically defined compounds, (ii) a C(4) leaf spiked with C(3) starch, and (iii) two natural plant samples (root, leaf). Starch preparation methods based on enzymatic or acid hydrolysis did not yield similar results and exhibited contaminations by non-starch compounds. The specificity of the acidic hydrolysis method was especially low, and we therefore suggest terming these preparations as HCl-hydrolysable carbon, rather than starch. Despite being more specific, enzyme-based methods to isolate starch also need to be further optimized to increase specificity. The analysis of sugars by ion-exchange methods (bulk preparations) was fast but produced more variable isotope compositions than compound-specific methods. Compound-specific approaches did not in all cases correctly reproduce the target values, mainly due to unsatisfactory separation of sugars and background contamination. Our study demonstrates that, despite their wide application, methods for the preparation of starch and soluble sugars for the analysis of carbon isotope composition are not (yet) reliable enough to be routinely applied and further research is urgently needed to resolve the identified problems. Copyright (C) 2009 John Wiley & Sons, Ltd.
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| 17. |
- Heim, C, et al.
(författare)
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Spectral characterisation of eight glycerolipid standards and detection in natural samples using time-of-flight secondary iion mass spectrometry
- 2009
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Ingår i: Rapid Communications in Mass Spectrometry. - 0951-4198 .- 1097-0231. ; 23:17, s. 2741-2753
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Tidskriftsartikel (refereegranskat)abstract
- In recent years, time-of-flight secondary ion mass spectrometry (ToF-SIMS) with cluster ion sources has opened new perspectives for the analysis of lipid biomarkers in geobiology and organic geochemistry. However, published ToF-SIMS reference spectra of relevant compounds are still sparse, and the influence of the chemical environment (matrix) on the ionisation of molecules and their fragmentation is still not well explored. This study presents ToF-SIMS spectra of eight glycerolipids as common target compounds in biomarker studies, namely ester- and ether-bound phosphatidylethanolamine, ester- and ether-bound phosphatidylcholine, ester-bound phosphatidylcholine, ester- and ether-bound diglycerides and archaeol, obtained with a Bi 3 + cluster ion source. For all of these compounds, the spectra obtained in positive and negative analytical modes showed characteristic fragments that could clearly be assigned to e.g. molecular ions, functional groups and alkyl chains. By comparison with the reference spectra, it was possible to track some of these lipids in a pre-characterised organic extract and in cryosections of microbial mats. The results highlight the potential of ToF-SIMS for the laterally resolved analysis of organic biomarkers in environmental materials. The identification of the target compounds, however, may be hampered by matrix effects (e.g. adduct formation) and often require careful consideration of all spectral features and taking advantage of the molecular imaging capability of ToF-SIMS.
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| 18. |
- Hyodo, Fujio, et al.
(författare)
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Effect of ecosystem retrogression on stable nitrogen and carbon isotopes of plants, soils and consumer organisms in boreal forest islands
- 2009
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Ingår i: Rapid Communications in Mass Spectrometry. - : Wiley. - 0951-4198 .- 1097-0231. ; 23, s. 1892-1898
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Tidskriftsartikel (refereegranskat)abstract
- In the prolonged absence of catastrophic disturbance, ecosystem retrogression occurs, and this involves increased nutrient limitation, and reduced aboveground and belowground ecosystem processes rates. Little is known about how the nitrogen and carbon stable isotope ratios (delta(15)N and delta(13)C) of plants, soils and consumer organisms respond to retrogression in boreal forests. We investigated a 5000 year chronosequence of forested islands in the boreal zone of northern Sweden, for which the time since lightning-induced wildfire increases with decreasing island size, leading to ecosystem retrogression. For this system, tissue delta(15)N of three abundant plant species (Betula pubescens, Vaccinium myrtillus and Pleurozium schreberi) and humus all increased as retrogression proceeded. This is probably due to enhanced ecosystem inputs of N by biological fixation, and greater dependency of the plants on organic N during retrogression. The delta(13)C of B. pubescens and plant-derived humus also increased during retrogression, probably through nutrient limitation increasing plant physiological stress. Unlike the plants, delta(15)N of invertebrates (lycosid spiders and ants) did not increase during retrogression, probably because of their partial dependence on aquatic-derived prey that had a variable delta(15)N signature. The delta(13)C of the invertebrates increased as retrogression proceeded and converged towards that of an aquatic prey source (chironomid flies), suggesting increased dependence on aquatic-derived prey during retrogression. These results show that measurement of delta(15)N and delta(13)C of plants, soils, and consumers across the same environmental gradient can provide insights into environmental factors that drive both the aboveground and belowground subsystems, as well as the linkages between them. Copyright (C) 2009 John Wiley & Sons, Ltd.
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| 19. |
- Jansson, Britt, et al.
(författare)
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Enantiospecific separation and quantitation of mephenytoin and its metabolites nirvanol and 4'-hydroxymephenytoin in human plasma and urine by liquid chromatography/tandem mass spectrometry
- 2006
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Ingår i: Rapid Communications in Mass Spectrometry. - : Wiley. - 0951-4198 .- 1097-0231. ; 20:3, s. 463-572
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Tidskriftsartikel (refereegranskat)abstract
- A sensitive method using enantiospecific liquid chromatography/tandem mass spectrometry detection for the quantitation of S- and R-mephenytoin as well as its metabolites S- and R-nirvanol and S- and R-4'-hydroxymephenytoin in plasma and urine has been developed and validated. Plasma samples were prepared by protein precipitation with acetonitrile, while urine samples were diluted twice with the mobile phase before injection. The analytes were then separated on a chiral alpha(1)-acid glycoprotein (AGP) column and thereafter detected, using electrospray ionization tandem mass spectrometry. In plasma, the lower limit of quantification (LLOQ) was 1 ng/mL for S- and R-4'-hydroxymephenytoin and S-nirvanol and 3 ng/mL for R-nirvanol and S- and R-mephenytoin. In urine, the LLOQ was 3 ng/mL for all compounds. Resulting plasma and urine intra-day precision values (CV) were <12.4% and <6.4%, respectively, while plasma and urine accuracy values were 87.2-108.3% and 98.9-104.8% of the nominal values, respectively. The method was validated for plasma in the concentration ranges 1-500 ng/mL for S- and R-4'-hydroxymephenytoin, 1-1000 ng/mL for S-nirvanol, and 3-1500 ng/mL for R-nirvanol and S- and R-mephenytoin. The validated concentration range in urine was 3-5000 ng/mL for all compounds. By using this method, the metabolic activities of two human drug-metabolizing enzymes, cytochrome P450 (CYP) 2C19 and CYP2B6, were simultaneously characterized.
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| 20. |
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| 21. |
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| 22. |
- Lampinen Salomonsson, Matilda, et al.
(författare)
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Structural evaluation of the glucuronides of morphine and formoterol using chemical derivatization with 1,2-dimethylimidazole-4-sulfonyl chloride and liquid chromatography/ion trap mass spectrometry
- 2008
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Ingår i: Rapid Communications in Mass Spectrometry. - : Wiley. - 0951-4198 .- 1097-0231. ; 22:17, s. 2685-2697
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Tidskriftsartikel (refereegranskat)abstract
- For the first time chemical derivatization of isomeric drug glucuronides with 1,2-dimethylimidazole-4-sulfonyl chloride (DMISC) has been successfully applied as a tool for determining the site of conjugation. This provides a way to differentiate between glucuronide isomers containing aliphatic and phenolic hydroxyl groups. The analyses were performed with liquid chromatography/electrospray ion trap mass spectrometry (LC/ESI-MSn). DMISC has previously been shown to react selectively with phenols in estrogens, thus improving sensitivity in ESI-MS. The model compounds selected for this study were commercially available standards of formoterol, morphine, morphine-3-glucuronide (M3G), and morphine-6-glucuronide (M6G). Formoterol glucuronides were produced with an enzymatic method in house. Both formoterol and morphine possess one phenolic and one aliphatic hydroxyl group where glucuronidation could take place. The product ion mass spectra of the native morphine glucuronides were indistinguishable due to the initial neutral loss of monodehydrated glucuronic acid (1.76u). However, a significant difference between the isomers was observed with DMISC derivatization, as only the form with a free phenol, M6G, gave a detectable reaction product. Formoterol formed two detectable glucuronide isomers in the enzymatic reaction. Their respective sites of conjugation could not be directly determined from the product ion spectra. Reaction with DMISC, however, gave a detectable product with only one of the isomers. Based on previous experience of the preferred DMISC reactions with phenols, and interpretation of the fragmentation pattern of the derivative, it was concluded that the reactive isomer had a free phenol, and was thus conjugated on the aliphatic chain.
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| 23. |
- Laumer, W., et al.
(författare)
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A novel approach for the homogenization of cellulose to use micro-amounts for stable isotope analyses
- 2009
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Ingår i: Rapid Communications in Mass Spectrometry. - : Wiley. - 0951-4198 .- 1097-0231. ; 23:13, s. 1934-1940
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Tidskriftsartikel (refereegranskat)abstract
- Climate reconstructions using stable isotopes from tree-rings are steadily increasing. The investigations concentrate mostly on cellulose due to its high stability. In recent years the available amount of cellulose has steadily decreased, mainly because micro-structures of plant material have had to be analyzed. Today, the amounts of cellulose being studied are frequently in the milligram and often in the microgram range. Consequently, homogeneity problems with regard to the stable isotopes of carbon and oxygen from cellulose have occurred and these have called for new methods in the preparation of cellulose for reliable isotope analyses. Three different methods were tested for preparing isotopically homogenous cellulose, namely mechanical grinding, freezing by liquid nitrogen with subsequent milling and ultrasonic breaking of cellulose fibres. The best precision of isotope data was achieved by freeze-milling and ultrasonic breaking. However, equipment for freeze-milling is expensive and the procedure is labour-intensive. Mechanical grinding resulted in a rather high loss of material and it is also labour-intensive. The use of ultrasound for breaking cellulose fibres proved to be the best method in terms of rapidity of sample throughput, avoidance of sample loss, precision of isotope results, ease of handling, and cost.
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| 24. |
- Li, Jianjun, et al.
(författare)
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Structural characterization of sialylated glycoforms of H-influenzae by electrospray mass spectrometry : fragmentation of protonated and sodiated O-deacylated lipopolysaccharides
- 2007
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Ingår i: Rapid Communications in Mass Spectrometry. - : Wiley. - 0951-4198 .- 1097-0231. ; 21:6, s. 952-960
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Tidskriftsartikel (refereegranskat)abstract
- Sialylated lipopolysaccharide (LPS) glycoforms from Haemophilus influenzae were characterized by tandem mass spectrometry using a new generation hyphenated mass spectrometer which combines a triple quadrupole and a linear ion trap (Q-Trap). The fragmentation of both protonated and sodiated molecular ions from O-deacylated LPS (LPS-OH) obtained in MS2 experiments in the positive mode was studied. The MS2 spectra of protonated ions provided unambiguous evidence for the presence and sequence of sialylated lactosamine present in lacto-N-neotetraose oligosaccharide extensions but not for sialyl-lactose structures whilst fragmentation of sodiated adducts, [M+Na](+), afforded information diagnostic of mono- and disialylated lactose extensions. To study this we used a highly sialylated LPS from a H. influenzae strain capable of sialyl-lactose expression only. We then applied the method to the H. influenzae genome strain, Rd, in which glycoforms containing both sialyl-lactose and sialyl-lacto-N-neotetraose were detected from diagnostic B-ions at m/z 638.2 ([Neu5Ac(1) Hex(2)+ Na](+)) and 657.2 ([Neu5Ac(1) Hex(1) HexNAc(1)+H](+)). Unique fragmentation patterns provided the locations and sequences of these oligosaccharide extensions. This is the first time both sialylated lactose and sialylated lacto-N-neotetraose units have been detected and characterized by tandem mass spectrometry in the same molecule. This methodology is of general applicability for determination of common sialylated oligosaccharide extension in bacterial LPS.
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| 25. |
- Lindh, Christian, et al.
(författare)
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Analysis of 3,5-dichloroaniline as a biomarker of vinclozolin and iprodione in human urine using liquid chromatography/triple quadrupole mass spectrometry.
- 2007
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Ingår i: Rapid Communications in Mass Spectrometry. - : Wiley. - 1097-0231 .- 0951-4198. ; 21:4, s. 536-542
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Tidskriftsartikel (refereegranskat)abstract
- The fungicides vinclozolin and iprodione are widely used in agriculture. These pesticides are dicarboximide fungicides containing the common moiety 3,5-dichloroaniline (3,5-DCA). It ha; been suggested that low-level exposures to such compounds may be associated with adverse health effects such as endocrine disruption. In this study a method using liquid chromatography/triple quadrupole mass spectrometry (LC/MS/MS) was developed for the analysis of 3,5-DCA as a biomarker of exposure to these fungicides in human urine. The urine samples were treated by basic hydrolysis to degrade the fungicides, their metabolites and conjugates to 3,5-DCA. The 3,5-DCA was then extracted using toluene and derivatized using pentafluoropropionic anhydride (PFPA). Analysis of the derivative was carried out using selected reaction monitoring (SRM) in the negative ion mode. Quantification of the derivative was performed using [C-13(6)]-labeled 3,4-DCA as an internal standard with good precision and linearity in the range 0.1-200 ng/mL urine. The limit of detection was determined to be 0.1 ng/mL. The metabolites in urine were found to be stable during storage at -20 degrees C. To validate 3,5-DCA as a biomarker the method was applied in a human experimental exposure to iprodione and vinclozolin. Two healthy volunteers received 200 jig single oral doses of each pesticide followed by urine sampling during 72-120 h post-exposure. Between 78-107% of the dose was recovered as 3,5-DCA in the urine after exposure.
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| 26. |
- Lindh, Christian, et al.
(författare)
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Analysis of ethylenethiourea as a biomarker in human urine using liquid chromatography/triple quadrupole mass spectrometry.
- 2008
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Ingår i: Rapid Communications in Mass Spectrometry. - : Wiley. - 1097-0231 .- 0951-4198. ; 22:16, s. 2573-2579
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Tidskriftsartikel (refereegranskat)abstract
- Ethylenebisdithiocarbamates (EBDCs) are widely used fungicides. Ethylenethiourea (ETU), the main metabolite and also a contaminant in the commercially available products, is of major toxicological concern. In this study, a method using liquid chromatography/triple quadrupole mass spectrometry (LC/MS/MS) is described for the analysis of ETU in human urine after a single-step extractive derivatization using pentafluorobenzyl bromide (PFBBr). Analysis was carried out using selected reaction monitoring (SRM) in the positive ion mode. Quantification of ETU was performed using [(2)H(4)]-labeled ETU as internal standard (IS). The limit of detection (LOD) was determined to 0.05 ng/mL. The method was linear in the range 0.1-54 ng/mL urine and had a within-run precision of 3-5%. The between-run precision was determined at an average urine level of 2 and 10 ng/mL urine and found to be 9%. The inter-batch precision was 6%. To validate ETU as a biomarker of exposure, the method was applied in a human experimental oral exposure to the commercial fungicide Ridomil Gold, containing 64% mancozeb and 4.5% ETU. Two healthy volunteers received 8.9 microg/kg body weight (b.w.) Ridomil Gold in a single oral dose followed by urine sampling for 104 h post-exposure. The elimination half-life of ETU was estimated to 17-23 h.
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| 27. |
- Lindh, Christian, et al.
(författare)
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Analysis of phenoxyacetic acid herbicides as biomarkers in human urine using liquid chromatography triple quadrupole mass spectrometry.
- 2008
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Ingår i: Rapid Communications in Mass Spectrometry. - : Wiley. - 1097-0231 .- 0951-4198. ; 22:2, s. 143-150
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Tidskriftsartikel (refereegranskat)abstract
- Phenoxyacetic acids are widely used herbicides. The toxicity of phenoxyacetic acids is debated, but high-level exposure has been shown to be hepatotoxic as well as nephrotoxic in animal studies. An inter-species difference in toxic effects has been found, with dogs particularly susceptible. In this study a method using liquid chromatography/triple quadrupole mass spectrometry (LC/MS/MS) is described for the analysis of 4-chloro-2-methylphenoxyacetic acid (MCPA), and its metabolite 4-chloro-2-hydroxymethylphenoxyacetic acid (HMCPA), 2,4-dichlorophenoxyacetic acid (2,4-D), and 2,4,5-trichlorophenoxyacetic acid (2,4,5-T) in human urine. The urine samples were treated by acid hydrolysis to degrade possible conjugations. The sample preparation was performed using solid-phase extraction. Analysis was carried out using selected reaction monitoring (SRM) in the negative ion mode. Quantification of the phenoxyacetic acids was performed using [2H3]-labeled MCPA and 2,4-D as internal standards. The method was linear in the range 0.05-310 ng/mL urine and has a within-run precision of 2-5%. The between-run precision in lower concentration ranges was between 6-15% and between 2-8% in higher concentration ranges. The limit of detection was determined to 0.05 ng/mL. The metabolites in urine were found to be stable during storage at -20°C. To validate the phenoxyacetic acids as biomarkers of exposure, the method was applied in a human experimental oral exposure to MCPA, 2,4-D and 2,4,5-T. Two healthy volunteers received 200 µg of each phenoxyacetic acid in a single oral dose followed by urine sampling for 72 h post-exposure. After exposure, between 90 and 101% of the dose was recovered in the urine. In the female subject, 23%, and in the male subject 17%, of MCPA was excreted as HMCPA.
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| 28. |
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| 29. |
- Malmberg, Per, 1974, et al.
(författare)
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Analysis of bone minerals by time-of-flight secondary ion mass spectrometry: a comparative study using monoatomic and cluster ions sources.
- 2007
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Ingår i: Rapid communications in mass spectrometry : RCM. - : Wiley. - 0951-4198 .- 1097-0231. ; 21:5, s. 745-9
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Tidskriftsartikel (refereegranskat)abstract
- Time-of-flight secondary ion mass spectrometry (TOF-SIMS) is an important tool for the analysis of bone minerals at implant surfaces. Most studies have been performed with monoatomic primary ion sources such as Ga(+) with poor secondary molecular ion production efficiency and only elemental distributions and minor fragments of bone minerals have been reported. By using cluster ion sources, such as Au(1-3) (+) and Bi(1-3) (+), identification of larger hydroxyapatite species at m/z 485, 541, 597 and 653, identified as Ca(5)P(3)O(12), Ca(6)P(3)O(13), Ca(7)P(3)O(14) and Ca(8)P(3)O(15), respectively, became possible. The ions appear to be fragments of the hydroxyapatite unit cell Ca(10)(PO(4))(6)(OH)(2). Each ion in the series is separated by 55.9 m/z units, corresponding to CaO, and this separation might reflect the columnar nature of the unit cell.
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| 30. |
- Misharin, Alexander S., et al.
(författare)
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Coaxial multi-electrode cell (' O-trap ') for high-sensitivity detection at a multiple frequency in Fourier transform ion cyclotron resonance mass spectrometry : main design and modeling results
- 2006
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Ingår i: Rapid Communications in Mass Spectrometry. - : Wiley. - 0951-4198 .- 1097-0231. ; 20:21, s. 3223-3228
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Tidskriftsartikel (refereegranskat)abstract
- Separation of the functions of ion excitation and detection between different cell compartments allows for implementation of excitation and detection techniques unattainable in a single compartment of the conventional ion cyclotron resonance (ICR) cell. In particular, multi-electrode detection at a multiple of the main cyclotron frequency can be utilized without the loss of sensitivity and other negative effects. The new O-trap designed exclusively for ion detection adds an additional, internal coaxial cylinder around which ions with excited cyclotron orbits rotate. Comparison of simulated performance characteristics of the new O-trap with those of the same-size conventional cylindrical cell shows that the O-trap can provide higher sensitivity and ion capacity. Multiplexing of the O-traps can further increase the analysis speed. Future efforts will be aimed at building and testing experimentally the coaxial O-trap, including optimization of the method of ion transfer between the compartments of the cell.
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| 31. |
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| 32. |
- Momcilovic, Dane, et al.
(författare)
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Improved matrix-assisted laser desorption/ionisation sample preparation of a partially depolymerised cellulose derivative by continuous spray deposition and interfacing with size-exclusion chromatography
- 2005
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Ingår i: Rapid Communications in Mass Spectrometry. - : Wiley. - 0951-4198 .- 1097-0231. ; 19:7, s. 947-954
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Tidskriftsartikel (refereegranskat)abstract
- Continuous spray deposition (CSD) of aqueous solutions of partially depolymerised methyl cellulose was found to improve matrix-assisted laser desorption/ionisation (MALDI) sample preparation. One feature was that the sensitivity in MALDI time-of-flight mass spectrometry increased up to an order of magnitude compared with the standard sample preparation method. Another feature was that CSD provided targets for MALDI with homogeneously distributed analyte. This resulted in a more even signal intensity and a higher reproducibility than in the standard method. High-mass discrimination was more pronounced in CSD than in the standard method. Size-exclusion chromatography with aqueous eluent was coupled online to CSD onto matrix-precoated foils. The suitability for determination of the molar mass distribution of methyl cellulose was investigated.
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| 33. |
- Nilsson, Johanna, 1984, et al.
(författare)
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Evaluation of ionization techniques for mass spectrometric detection of contact allergenic hydroperoxides formed by autoxidation of fragrance terpenes.
- 2008
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Ingår i: Rapid communications in mass spectrometry : RCM. - : Wiley. - 0951-4198. ; 22:22, s. 3593-8
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Tidskriftsartikel (refereegranskat)abstract
- Hydroperoxides formed by autoxidation of common fragrance terpenes are strong allergens and known to cause allergic contact dermatitis (ACD), a common skin disease caused by low molecular weight chemicals. Until now, no suitable methods for chemical analyses of monoterpene hydroperoxides have been available. Their thermolability prohibits the use of gas chromatography and their low UV-absorption properties do not promote sensitive analytical methods by liquid chromatography based on UV detection. In our study, we have investigated different liquid chromatography/mass spectrometry (LC/MS) ionization techniques, electrospray ionization (ESI), atmospheric pressure chemical ionization (APCI), and atmospheric pressure photoionization (APPI), for detection of hydroperoxides from linalool and limonene.Flow injection analysis was used to evaluate the three different techniques to ionize the monoterpene hydroperoxides, linalool hydroperoxide and limonene hydroperoxide, by estimating the signal efficacy under experimental conditions for positive and negative ionization modes. The intensities for the species [M+H](+) and [M+H-H(2)O](+) in positive ionization mode and [M-H](-) and [M-H-H(2)O](-) in negative ionization mode were monitored. It was demonstrated that the mobile phase composition and instrumental parameters have major influences on the ionization efficiency of these compounds. ESI and APCI were both found to be appropriate as ionization techniques for detection of the two hydroperoxides. However, APPI was less suitable as ionization technique for the investigated hydroperoxides. Copyright (c) 2008 John Wiley & Sons, Ltd.
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| 34. |
- Osman, Abdimajid, et al.
(författare)
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A possible ethanol-catalyzed rearrangement of vitamin K-1 detected by gas chromatography/mass spectrometry
- 2008
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Ingår i: Rapid Communications in Mass Spectrometry. - : Wiley. - 0951-4198 .- 1097-0231. ; 22:23, s. 3861-3866
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Tidskriftsartikel (refereegranskat)abstract
- We studied vitamin K-1(20), vitamin K-1(25), and vitamin K, epoxide in n-hexane and ethanol solutions by gas chromatography/mass spectrometry (GC/MS) utilizing a DB-5 MS fused-silica capillary column. In ethanol solutions of K-1, we observed an extra peak eluting from the GC column with somewhat longer retention time than K-1(20). A similar peak following K-1(25) was also found. These peaks were not found in n-hexane solutions of K-1. A close examination of the mass spectra of these peaks indicated that they were vitamin K-1 variants containing a base peak at m/z 225 characteristic of the methylnaphthoquinone ring with a four-carbon side chain. In addition, they contained the molecular ions of K-1(20) and K-1(25), respectively. We conclude that K-1(20) and K-1(25), but not K-1 epoxide, might undergo rearrangements in ethanol involving an intramolecular proton transfer and a shift of the beta,gamma-double bond on the phytyl side chain toward the ring. The conjugation of the phytyl double bond with the quinone ring is probably the driving force of the rearrangement. We emphasize, however, that our conclusion is based only on mass spectral analysis and would require further investigation by other spectroscopic methods.
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| 35. |
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| 36. |
- Salehpour, Mehran, et al.
(författare)
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Accelerator mass spectrometry of small biological samples
- 2008
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Ingår i: Rapid Communications in Mass Spectrometry. - : Wiley. - 0951-4198 .- 1097-0231. ; 22:23, s. 3928-3934
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Tidskriftsartikel (refereegranskat)abstract
- Accelerator mass spectrometry (AMS) is an ultra-sensitive technique for isotopic ratio measurements. In the biomedical field, AMS can be used to measure femtomolar concentrations of labeled drugs in body fluids, with direct applications in early drug development such as Microdosing. Likewise, the regenerative properties of cells which are of fundamental significance in stem-cell research can be determined with an accuracy of a few years by AMS analysis of human DNA. However, AMS nominally requires about 1 mg of carbon per sample which is not always available when dealing with specific body substances such as localized, organ-specific DNA samples. Consequently, it is of analytical interest to develop methods for the routine analysis of small samples in the range of a few tens of mu g. We have used a 5 MV Pelletron tandem accelerator to study small biological samples using AMS. Different methods are presented and compared. A 12 C-carrier sample preparation method is described which is potentially more sensitive and less susceptible to contamination than the standard procedures.
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| 37. |
- Salehpour, Mehran, et al.
(författare)
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FemtoMolar measurements using accelerator mass spectrometry
- 2009
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Ingår i: Rapid Communications in Mass Spectrometry. - : Wiley. - 0951-4198 .- 1097-0231. ; 23:5, s. 557-563
-
Tidskriftsartikel (refereegranskat)abstract
- Accelerator mass spectrometry (AMS) is an ultra-sensitive analytical method suitable for the detection of sub-nM concentrations of labeled biological substances such as pharmaceutical drugs in body fluids. A limiting factor in extending the concentration measurements to the sub-pM range is the natural C-14 content in living tissues. This was circumvented by separating the labeled drug from the tissue matrix, using standard high-performance liquid chromatography (HPLC) procedures. As the separated total drug amount is in the few fg range, it is not possible to use a standard AMS sample preparation method, where mg sizes are required. We have utilized a sensitive carbon carrier method where a C-14-deficient compound is added to the HPLC fractions and the composite sample is prepared and analyzed by AMS. Using 50 mu L human blood plasma aliquots, we have demonstrated concentration measurements below 20 JFM, containing sub-amol amounts of the labeled drug. The method has the immediate potential of operating in the sub-fM region.
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| 38. |
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| 39. |
- Samgina, Tatiana Yu., et al.
(författare)
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De novo sequencing of peptides secreted by the skin glands of the Caucasian Green Frog Rana ridibunda
- 2008
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Ingår i: Rapid Communications in Mass Spectrometry. - : Wiley. - 0951-4198 .- 1097-0231. ; 22:22, s. 3517-3525
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Tidskriftsartikel (refereegranskat)abstract
- Amphibian skin glands are known to secrete various types of bioactive peptides. The array of these peptides is specific for every frog species. The present research deals with the identification of peptides isolated from the skin secretion of the Marsh frog R. ridibunda inhabiting the Kolkhida Canyon of the Caucasian region. The research is based on comprehensive high-performance liquid chromatography/tandem mass spectrometry (HPLC/MS/MS) analysis of intact and chemically modified peptides. In particular, an oxidation procedure was applied directly to the crude skin secretion to open S-S loops whereas N-terminal acetylation was additionally carried out for one individual peptide. Sequences were determined by manual interpretation of electron capture dissociation (ECD) and collisionally induced dissociation (CID) tandem mass spectra. A total of 29 peptides were identified in the skin secretion of the Caucasian Marsh frog. The peptide profile is represented with disulfide-containing peptides belonging to the brevinin, esculentin and ranatuerin families, neuropeptides of the bradykinin and bombesin families. Two identified peptides belonging to the ranatuerins are the first peptides of this family discovered in the skin secretions of European frogs. Ten of the identified peptides coincide with those reported earlier for the European Edible frog. Another ten are identical to those found in R. ridubunda from the Moscow region. This fact verifies the described method as being art efficient analytical tool to compare intra- and interspecific variabilities.
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| 40. |
- Shariatgorji, Mohammadreza, et al.
(författare)
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Matrix-free thin-layer chromatography/laser desorption ionization mass spectrometry for facile separation andidentification of medicinal alkaloids
- 2009
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Ingår i: Rapid Communications in Mass Spectrometry. - : Wiley. - 0951-4198 .- 1097-0231. ; 23:23, s. 3655-3660
-
Tidskriftsartikel (refereegranskat)abstract
- Quaternary protoberberine alkaloids belong to a pharmaceutically important class of isoquinoline alkaloids associated with bactericidal, fungicidal, insecticidal and antiviral activities. As traditional medicine gains wider acceptance, quick and robust analytical methods for the screening and analysis of plants containing these compounds attract considerable interest. Thin-layer chromatography (TLC) combined with matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS) is a powerful technique but suffers from dilution of the TLC bands resulting in decreased sensitivity and masking of signals in the low-mass region both due to addition of matrix. This study integrates for the first time conventional silica gel TLC and laser desorption ionization mass spectrometry (LDI-MS) thus eliminating the need for any external matrix. Successful separation of berberine (Rf = 0.56) and palmatine (Rf = 0.46) from Berberis barandana including their identification by MS are demonstrated. Furthermore, a robust electrospray ionization (ESI)-MS method utilizing residual sample from TLC for quantification of berberine applying selected reaction monitoring and standard addition method is presented. The amount of berberine in the plant root prepared for the study was determined to be 0.70% (w/w). Copyright © 2009 John Wiley & Sons, Ltd.
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| 41. |
- Spacil, Zdenek, et al.
(författare)
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Matrix-less laser desorption/ionisation mass spectrometry of polyphenols in red wine
- 2009
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Ingår i: Rapid Communications in Mass Spectrometry. - : Wiley. - 0951-4198 .- 1097-0231. ; 23:12, s. 1834-1840
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Tidskriftsartikel (refereegranskat)abstract
- Matrix-assisted laser desorption/ionisation (MALDI) of small molecules is challenging and in most cases impossible due to interferences from matrix ions precluding analysis of molecules <300-500 Da. A common matrix such as ferulic acid belongs to an important class of compounds associated with antioxidant activity. If the shared phenolic structure is related to the propensity as an active MALDI matrix then it follows that direct laser desorption/ionisation should be possible for polyphenols. Indeed matrix-less laser desorption/ionisation mass spectrometry is achieved whereby the analyte functions as a matrix and was used to monitor low molecular weight compounds in wine samples. Sensitivity ranging from 0.12-87 pmol/spot was achieved for eight phenolic acids (4-coumaric, 4-hydroxybenzoic, caffeic, ferulic, gallic, protocatechuic, syringic, vanillic) and 0.02 pmol/spot for trans-resveratrol. Additionally, 4-coumaric, 4-hydroxybenzoic, caffeic, ferulic, gallic, syringic, vanillic acids and trans-resveratrol were identified in wine samples using accurate mass measurements consistent with reported profiles based on liquid chromatography (LC)/MS. Minimal sample pre-treatment make the technique potentially appropriate for fingerprinting, screening and quality control of wine samples. Copyright © 2009 John Wiley & Sons, Ltd.
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| 42. |
- Sundqvist, Gustav, et al.
(författare)
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Investigation of multiple binding sites on ribonuclease A using nano-electrospray ionization mass spectrometry
- 2005
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Ingår i: Rapid Communications in Mass Spectrometry. - : Wiley. - 0951-4198 .- 1097-0231. ; 19:8, s. 1011-1016
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Tidskriftsartikel (refereegranskat)abstract
- Multiple non-active site interactions between ribonuclease A (RNAse) and selected target molecules were investigated using nano-electrospray ionization mass spectrometry (nano-ESI-MS). Among the building blocks of RNA, phosphate and ribose showed such multiple interactions. Multiple phosphate interactions survived a high cone voltage, while multiple interactions with D-ribose disappeared already at a low cone voltage. Using nano-ESI-MS, only cytosine among the individual bases appeared to interact with RNAse. Interestingly, guanosine binds to the RNAse surface at high cone voltage, probably as a result of cooperative binding of the sugar and the guanine base. Upon binding of deoxycytidine oligonucleotides with six (dC(6)), nine (dC(9)) and twelve (dC(12)) deoxycytidine nucleotide units to RNAse, the dC(12) Unit showed the strongest interaction. Upon collision-induced dissociation (CID) of the RNAse/dC(6) complex, this complex survived dissociation at an energy level where covalently bound cytosine from dC(6) was lost. This is in contrast to CID of RNAse complexed with mononucleotide cytidine 2'-monophosphate (CMP), which dissociates from the protein without breaking of covalent bonds.
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| 43. |
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| 44. |
- Törnvall, Ulrika, et al.
(författare)
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Mass spectrometric analysis of peptides from an immobilized lipase: focus on oxidative modifications.
- 2009
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Ingår i: Rapid Communications in Mass Spectrometry. - : Wiley. - 1097-0231 .- 0951-4198. ; 23:18, s. 2959-2964
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Tidskriftsartikel (refereegranskat)abstract
- Liquid chromatography/tandem mass spectrometry (LC/MS/MS) was used to study the primary structure of immobilized Candida antarctica lipase B (Novozym(R)435) without detaching the enzyme from the carrier. The immobilized enzyme packed in a miniature column was subjected to proteolysis and the peptides released were injected into the mass spectrometer for analysis. The set-up was utilized to determine amino acid oxidation after treatment of the biocatalyst with hydrogen peroxide. In total, sequence coverage of more than 90% was obtained, containing almost all of the amino acids sensitive to oxidation. Oxidation of methionine, tryptophan and cystine residues was observed. The flow system also allowed evaluation of the enzyme activity prior to peptide analysis. The developed method is general and should be applicable to other immobilized enzyme systems and to different treatments.
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| 45. |
- Wang, Lijun, 1979-, et al.
(författare)
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High-temperature mass spectrometric study of the vaporization process in the system CaO-MgO-Al2O3-Cr2O3-FeO-SiO2
- 2009
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Ingår i: Rapid Communications in Mass Spectrometry. - : Wiley. - 0951-4198 .- 1097-0231. ; 23, s. 2233-2239
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Tidskriftsartikel (refereegranskat)abstract
- Knudsen effusion mass spectrometry was used to study vaporization processes and thermodynamic properties of twenty samples of chromium-containing slags in the CaO-MgO-Al2O3-Cr2O3-FeO-SiO 2 system in the temperature range 1850-2750 K. Tungsten cells were used and Cr2O3 solid was used as a reference material. The system was calibrated using liquid gold. As FeO was the first emanating vapor species, monitoring of the chromium-containing species could be carried out only after the complete vaporization of FeO. This, however, was found to have very little impact on the concentration of the slags investigated. During the measurements, the ion current intensities of CrO+ and CrO +2 species in the mass spectra of the vapor over the CaO-MgO-Al2O3-Cr2O3-FeO-SiO 2 samples were monitored and compared with those corresponding to solid Cr2O3. Data on the partial pressures of vapor species as well as the activities of Cr2O3 as a function of temperature were obtained. The results are expected to be valuable in the optimization of slag composition in high alloy steelmaking processes.
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