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Method development for the analysis of complex samples with inductively coupled plasma mass spectrometry
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Chemistry - BMC, Analytical Chemistry.
2019 (English)Doctoral thesis, comprehensive summary (Other academic)
Description
Abstract [en]

In this thesis the development of methods for handling the problems associated with analyzing trace elements in complex matrixes using inductively coupled plasma mass spectrometry is presented. Trace elements such as Cu, Fe, Se, and Zn, to name a few, do play important roles in different organisms. Therefore it can be of importance to study trace elements in different samples of biological origin. As trace elements are low in abundance, sensitive instrumental techniques such as inductively coupled plasma mass spectrometry (ICP-MS) are required for accurate determination. Due to the complexity of samples with biological origin, careful method development, both regarding the sample preparation and instrumental analysis has to be performed to minimize negative effects on the instrument signal and introduction of interferences.

For example the metal contents of mink livers were analyzed, after bomb digestion to investigate if the metal concentration could be linked to changes in the organ morphology as well as the minks’ environment. Morphological changes and capture locations could be linked to the metals investigated. The investigation of the elemental composition of cerebrospinal fluid from chronic pain patients using spinal cord stimulation electrode treatment on the other hand required less harsh sample treatment. No correlation between the spinal cord stimulation and element concentration could be found, but differences between patients and the control group were presented hinting that chronic pain intrinsically could affect the cerebrospinal fluid metal concentration. Another bodily fluid of interest is saliva and the use of paperpoint sticks as a sampling technique for Ti in saliva was investigated. As Ti is interfered by several components expected to be found in saliva, the use of reaction or collision gas was also investigated to reduce the effects of interferences. Simple leaching of the paperpoint sticks together with complexing the Ti with NH3 as reaction gas was shown to be optimal. Finally, how the selection of internal standard would be affected by the use of reaction and collision gases was also investigated. With collision gas most internal standards worked fine, while for reaction gas internal standard selection was harder. For elements with high ionization energy such as As, Se and Zn the choice of internal standard was very dependent on matrix. While ICP-MS suffers from problems when analyzing samples with complex matrixes many of them can be minimized by proper method development as shown in this thesis.

Place, publisher, year, edition, pages
Uppsala: Acta Universitatis Upsaliensis, 2019. , p. 52
Series
Digital Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology, ISSN 1651-6214 ; 1865
Keywords [en]
ICP-MS, trace elements, complex matrix.
National Category
Analytical Chemistry
Identifiers
URN: urn:nbn:se:uu:diva-394936ISBN: 978-91-513-0772-5 (print)OAI: oai:DiVA.org:uu-394936DiVA, id: diva2:1360053
Public defence
2019-11-29, B41, BMC, Husargatan 3, Uppsala, 13:15 (English)
Opponent
Supervisors
Available from: 2019-11-08 Created: 2019-10-10 Last updated: 2019-11-08
List of papers
1. Heavy metal concentrations in female wild mink (Neovison vison) in Sweden: Sources of variation and associations with internal organ weights
Open this publication in new window or tab >>Heavy metal concentrations in female wild mink (Neovison vison) in Sweden: Sources of variation and associations with internal organ weights
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2017 (English)In: Environmental Toxicology and Chemistry, ISSN 0730-7268, E-ISSN 1552-8618, Vol. 36, no 8, p. 2030-2035Article in journal (Refereed) Published
Abstract [en]

The American mink is an invasive species in Sweden, and it is legally hunted all year. Therefore, the mink is well suited as a sentinel species for environmental monitoring. In the present study female mink (n = 91) from 6 different areas in Sweden were analyzed for the concentrations of silver, cadmium, mercury and lead in liver tissue using inductively coupled plasma mass spectrometry. The wet concentrations in liver tissue were 42.6 +/- 52.7 ng/g for silver, 99.5 +/- 100 ng/g for cadmium, 652 +/- 537 ng/g formercury, and 196 +/- 401 ng/g for lead (expressed as mean + standard deviation). There were associations between the sample area and the concentrations of silver, lead, and mercury. The concentrations of lead and cadmium varied with season of capture and lead, cadmium, and mercury were positively associated with increasing age. Relative liver weight was positively associated with concentrations of mercury and negatively associated with lead and cadmium. Relative kidney weight was negatively associated with lead concentrations. In summary, it is of importance to take age and season of capture into account when assessing levels of heavy metals in wild mink. Also, liver and kidneys seem to be potential targets for heavy metal toxicity in wild female mink in Sweden.

Keywords
Wildlife toxicology, Metal accumulation, Metal toxicity, Mink, Liver, Kidney
National Category
Environmental Sciences Pharmacology and Toxicology
Identifiers
urn:nbn:se:uu:diva-333514 (URN)10.1002/etc.3717 (DOI)000406398400011 ()
Available from: 2017-11-20 Created: 2017-11-20 Last updated: 2019-10-10Bibliographically approved
2. Quantification of 10 elements in human cerebrospinal fluid from chronic pain patients with and without spinal cord stimulation
Open this publication in new window or tab >>Quantification of 10 elements in human cerebrospinal fluid from chronic pain patients with and without spinal cord stimulation
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2016 (English)In: Journal of Trace Elements in Medicine and Biology, ISSN 0946-672X, E-ISSN 1878-3252, Vol. 37, p. 1-7Article in journal (Refereed) Published
Abstract [en]

Neuropathic pain affects 1-10% of the general population and is caused by a lesion or disease of the somatosensory nervous system. Spinal cord stimulation (SCS), a method where implanted electrodes stimulate the spinal cord, has been successfully used to treat drug-resistant neuropathic pain, but the mechanism of action is largely unknown. Studies show that SCS changes the protein levels in CSF (cerebrospinal fluid) of pain patients. Several neurological conditions have been shown to alter the elemental composition of CSF. Therefore changes in the levels of ions and trace elements in the CSF may correspond to SCS use. This study used ICP-MS (Inductively coupled plasma mass spectrometry) and ICP-AES (Inductively coupled plasma atomic emission spectroscopy) to quantify 10 elements in CSF from chronic neuropathic pain patients using SCS. The element concentrations in CSF from patients with SCS treatment on/off, were measured. No effect on the element concentrations in CSF from treatment with SCS could be detected. Also, the elemental concentrations in pooled CSF from patients without chronic neuropathic pain was determined and compared to the patients using SCS. The concentration of the elements Ca, Sr, Na, K, P, Mg and Ti were, significantly higher in patients compared to the CSF-control.

Keywords
Chronic pain, Spinal cord stimulation, ICP-MS, ICP-AES, Trace elements, CSF
National Category
Medical and Health Sciences
Identifiers
urn:nbn:se:uu:diva-304549 (URN)10.1016/j.jtemb.2016.06.003 (DOI)000381840800001 ()27473826 (PubMedID)
Available from: 2016-10-06 Created: 2016-10-06 Last updated: 2019-10-10Bibliographically approved
3. Development of a method using paperpoint stick sampling to determine Ti concentration in saliva with ICP-MS
Open this publication in new window or tab >>Development of a method using paperpoint stick sampling to determine Ti concentration in saliva with ICP-MS
(English)Manuscript (preprint) (Other academic)
Abstract [en]

Peri-implantitis is a disease that causes an inflammatory process in soft tissues as well as bone loss around dental implants integrated into bone. The relationship between peri-implantitis and titanium presence has previously been established and also a correlation between the inflammation severity and Ti concentration in biopsies from patients with dental implants. Biopsy can be considered as an invasive sampling procedure and therefore there is an interest to study alternative sampling methods, such as collecting saliva with paperpoint sticks. The small volume absorbed by the paperpoint sticks requires a sensitive detection method for Ti, therefore ICP-MS was used. To minimize the effect of common polyatomic interferences on Ti, the use of He as a collision gas and complexation using NH3 as reaction gas were investigated and both methods were compared to each other. Three sample preparation techniques were investigated: leaching, ultrasonic extraction and microwave bomb digestion. The use of paperpoint sticks for sampling was shown to be a valid approach with simple leaching in combination with ICP-MS using either He- or NH3-gas. The use of NH3-gas to create a 131Ti-complex, required more technical expertise, but gave a 2 times lower detection limit compared to using He as a collision gas.

National Category
Analytical Chemistry
Identifiers
urn:nbn:se:uu:diva-394935 (URN)
Available from: 2019-10-10 Created: 2019-10-10 Last updated: 2019-10-10
4. Internal standards in inductively coupled plasma mass spectrometry using kinetic energy discrimination and dynamic reaction cells
Open this publication in new window or tab >>Internal standards in inductively coupled plasma mass spectrometry using kinetic energy discrimination and dynamic reaction cells
2018 (English)In: Journal of Analytical Atomic Spectrometry, ISSN 0267-9477, E-ISSN 1364-5544, Vol. 33, no 10, p. 1770-1776Article in journal (Refereed) Published
Abstract [en]

ICP-MS is a sensitive element analysis technique used for analyzing several different sample types. This can result in difficult matrixes which can affect both physical parameters and create overlaps of analyte elements. Some of the possible overlaps can be reduced by the use of reaction and/or collision cells, while the use of internal standards can help with reducing the physical interferences caused by a matrix. While both internal standardization and the use of cells have been studied separately, their effects on each other have not been investigated earlier. In this study ICP-MS was used to analyze Mg-24, Al-27, Ti-47, Ti-49, V-51, Cr-52, Cr-53, Mn-55, Fe-57, Co-59, Ni-60, Ni-61, Ni-62, Cu-63, Cu-65, Zn-66, Zn-67, As-75, Se-78, Se-82, Cd-111, and Pb-208 with Be-9, Y-89, Ga-69, Rh-103, In-115, Ir-193, and Tl-205 as internal standards with high concentrations of either HNO3, PBS-buffer, or Triton X-100 as the matrix, in reaction-, collision- and standard-cell modes. This was done to investigate which internal standards would compensate matrix effects in different cell modes. All internal standards, except Be, compensated fairly well (relative sensitivity RSD < 10%) even for severe matrix effects for most elements regardless of similarity in mass in the different cell modes. For Zn, As and Se no proper internal standard could be found, of the ones investigated.

Place, publisher, year, edition, pages
ROYAL SOC CHEMISTRY, 2018
National Category
Analytical Chemistry
Identifiers
urn:nbn:se:uu:diva-369509 (URN)10.1039/c8ja00171e (DOI)000448340200019 ()
Available from: 2018-12-14 Created: 2018-12-14 Last updated: 2019-10-10Bibliographically approved

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