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Development and application of high-throughput methods for analysis of persistent organic pollutants in human blood
Örebro University, School of Science and Technology.ORCID iD: 0000-0001-5752-4196
2013 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

The general public is continuously exposed to a wide range of environmental pollutants. This thesis focuses on a group of anthropogenic chemicals referred to as persistent organic pollutants (POPs) that have been linked to various adverse health effects in humans.

The main objective of this thesis was focused on the development and application of high-throughput methods for analysis of a broad range of chlorinated, brominated, and fluorinated POPs in human blood.

After establishing that the methods were effective, the two methods were applied to human plasma samples to examine the background levels of a broad range of POPs in human plasma samples among elderly men and women from Sweden and to assess the influence of gender. Levels of a wide range of chlorinated, brominated, and fluorinated compounds were determined in plasma samples collected during 2001-2004 from 1, 016 (50.2% women) 70 year-old participants from the population-based Prospective Study of the Vasculature in Uppsala Seniors (PIVUS). The POPs studied were 16 polychlorinated biphenyls (PCBs), 5 organochlorine pesticides (OCPs), 1 dioxin, 1 brominated flame retardant as well as 14 perfluoroalkyl substances (PFAS) including structural perfluorooctane sulfonic acid (PFOS) isomers. The majority of the studied compounds were detected in the 70-100% of the participants. The structural PFOS isomers were successfully quantified in a sub-sample of 25 men and women. Furthermore, gender differences in the concentrations of the POPs studied showed that the majority of chlorinated and brominated compounds were significantly different when comparing men and women in the study, while the concentrations of the fluorinated compounds were found to be less influenced by gender.

This thesis has, by using the developed high-throughput methods requiring only small amounts of human blood, provided background exposure information of a broad range of POPs for an epidemiological study.

Place, publisher, year, edition, pages
Örebro: Örebro universitet , 2013. , p. 70
Series
Örebro Studies in Chemistry, ISSN 1651-4270 ; 12
Keywords [en]
Human blood, POPs, Perfluoroalkylated substances, Structural isomers, Sample preparation, Column-switch, Mass spectrometry
National Category
Chemical Sciences
Research subject
Chemistry
Identifiers
URN: urn:nbn:se:oru:diva-28456ISBN: 978-91-7668-936-3 (print)OAI: oai:DiVA.org:oru-28456DiVA, id: diva2:612574
Public defence
2013-05-31, Hörsal B, Billbergska huset, Örebro universitet, Fakultetsgatan 1, Örebro, 10:00 (English)
Opponent
Supervisors
Available from: 2013-03-22 Created: 2013-03-22 Last updated: 2017-10-17Bibliographically approved
List of papers
1. Trends in the analysis of persistent organic pollutants (POPs) in human blood
Open this publication in new window or tab >>Trends in the analysis of persistent organic pollutants (POPs) in human blood
2013 (English)In: TrAC. Trends in analytical chemistry, ISSN 0165-9936, E-ISSN 1879-3142, Vol. 46, p. 129-138Article in journal (Refereed) Published
Abstract [en]

The general demands on analytical practices in laboratories involved in monitoring concentrations of persistent organic pollutants (POPs) in human blood in the context of the Stockholm Convention are met by the validated analytical procedures applied in most laboratories today. At the same time, as the concentrations of many of the legacy POPs are decreasing in the general populations, more specific, sensitive, and accurate analytical techniques are required. Thus, a challenge for the Stockholm Convention is the analytical capacity, in terms of quality and availability worldwide, to monitor declining concentrations of POPs in human blood. However, other POP issues (e.g., those targeted by epidemiological studies) might require different information and therefore more specialized analytical procedures having greater instrumental sensitivity.

We review current and emerging analytical procedures used for analysis of the chlorinated, brominated, and fluorinated classes of POPs in human blood with a focus on the compounds included in the Stockholm Convention. In general, analytical trends in sample clean-up, separation, detection techniques and quality protocols provide a tool for POP laboratories to measure POPs in human blood. Techniques based on established mass-selective instruments are most commonly employed but declining concentrations in humans in the future might require more selective, more sensitive techniques.

Place, publisher, year, edition, pages
Oxon, UK: Elsevier, 2013
Keywords
Gas chromatography (GC), High-resolution mass spectrometry (HRMS), Human blood, Liquid chromatography (LC), Organochlorine (OC) pesticide, Perfluoroalkylated substance (PFAS), Polychlorinated biphenyl (PCB), Polychlorinated dibenzo-p-dioxin (PCDD), Polychlorinated diphenyl ether (PBDE), Stockholm Convention
National Category
Chemical Sciences Analytical Chemistry
Research subject
Chemistry
Identifiers
urn:nbn:se:oru:diva-29858 (URN)10.1016/j.trac.2012.06.009 (DOI)000319087800027 ()2-s2.0-84876816513 (Scopus ID)
Available from: 2013-06-28 Created: 2013-06-28 Last updated: 2017-12-06Bibliographically approved
2. A rapid method for screening of the Stockholm Convention POPs in small amounts of human plasma using SPE and HRGC/HRMS
Open this publication in new window or tab >>A rapid method for screening of the Stockholm Convention POPs in small amounts of human plasma using SPE and HRGC/HRMS
Show others...
2012 (English)In: Chemosphere, ISSN 0045-6535, E-ISSN 1879-1298, Vol. 86, no 7, p. 747-753Article in journal (Refereed) Published
Abstract [en]

A rapid analytical screening method allowing simultaneous analysis of 23 persistent organic pollutants (POPs) in human plasma was developed. Sample preparation based on solid-phase extraction (SPE) with additional clean-up using small multilayer silica gel columns. SPE was performed using a custom made polystyrene-divinylbenzene sorbent for the extraction of chlorinated and brominated POPs. Special efforts to reduce sample volume and improve speed and efficiency of the analytical procedure were made. Determination of 16 polychlorinated biphenyls (PCBs), 5 organochlorine (OC) pesticides, octachlorinated dibenzo-p-dioxin (OCDD) and polybrominated diphenyl ether (BDE #47) in 0.5 mL human plasma was performed by using high resolution gas chromatography coupled to high resolution mass spectrometry (HRGC/HRMS). Recovery of POPs ranged between 46% and 110%, and reproducibility was below 25% relative standard deviation (RSD) for all target compounds, except for trans-nonachlor and OCDD, which were present only at low levels. Limits of detection (LOD) were for the PCBs between 0.8 and 117.7 pg mL(-1) plasma and for the OC pesticides between 5.9 and 89.1 pg mL(-1) plasma. The LOD for OCDD and BDE #47 were 1.4 pg mL(-1) plasma, and 9.2 pg mL(-1) plasma, respectively. The presented method was successfully applied to 1016 human plasma samples from an epidemiological study on cardiovascular disease. (C) 2011 Elsevier Ltd. All rights reserved.

Place, publisher, year, edition, pages
Elsevier, 2012
Keywords
Persistent organic pollutants, Sample extraction, Human plasma, HRGC/HRMS, Polychlorinated biphenyls, Organochlorine pesticides
National Category
Chemical Sciences
Research subject
Environmental Chemistry
Identifiers
urn:nbn:se:oru:diva-22315 (URN)10.1016/j.chemosphere.2011.11.006 (DOI)000301166700008 ()22153485 (PubMedID)2-s2.0-84856031844 (Scopus ID)
Available from: 2012-04-02 Created: 2012-04-02 Last updated: 2017-12-07Bibliographically approved
3. A rapid method for analysis of PFAS including structural PFOS isomers in human serum using 96-well plate column-switching UPLC-S/MS
Open this publication in new window or tab >>A rapid method for analysis of PFAS including structural PFOS isomers in human serum using 96-well plate column-switching UPLC-S/MS
Show others...
(English)Manuscript (preprint) (Other academic)
Abstract [en]

To facilitate high-throughput analysis suitable for large epidemiological studies we developed an automated column-switching ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for determination of perfluorocarboxylates (PFCAs; C5, C6, C7, C8, C9, C10, C11, C12, and C13), perfluoroalkyl sulfonic acids (PFSAs; C4, C6, C8, and C10), perfluorooctane sulfonamide (PFOSA), and five groups of structural perfluorooctane sulfonic acids (PFOS) isomers in human serum or plasma. The analytical procedure involves rapid protein precipitation using 96-well plates followed by a fully automated sample clean-up using an on-line trap column removing many potentially interfering sample components while through the mobile phase gradient the target analytes are eluted onto the analytical column for further separation and subsequent mass detection. The method showed good linearity (R2 < 0.995) at concentrations ranging from 0.01 to 60 ngmL-1 and low method detection limits (MDLs) ranging between 0.01-0.17 ngmL-1 depending on the analyte. The precision of the developed method was good, with within-run (n=7) and between-run (n=103) coefficients of variation between 2% and 20% for most compounds including PFOS (2%, 8%) and its structural isomers (2-6% and 4-8%). The method showed good conformity with a standard reference material (n=56). The columnswitching UPLC method has been successfully applied for the determination of perflourinated alkyl acids (PFAAs), including structural PFOS isomers, and PFOSA in human plasma from an epidemiological study.

Keywords
human blood, perfluoroalkylated substances, structural isomers, perfluorooctane sulfonamide, sample preparation, column-switch, pfos, pfoa
National Category
Chemical Sciences
Research subject
Chemistry
Identifiers
urn:nbn:se:oru:diva-30109 (URN)
Available from: 2013-08-02 Created: 2013-08-02 Last updated: 2017-10-17Bibliographically approved
4. Circulating levels of Persistent Organic Pollutants (POPs) among elderly men and women from Sweden: results from the Prospective Investigation of the Vasculature in Uppsala Seniors (PIVUS)
Open this publication in new window or tab >>Circulating levels of Persistent Organic Pollutants (POPs) among elderly men and women from Sweden: results from the Prospective Investigation of the Vasculature in Uppsala Seniors (PIVUS)
Show others...
2012 (English)In: Environment International, ISSN 0160-4120, E-ISSN 1873-6750, Vol. 44, p. 59-67Article in journal (Refereed) Published
Abstract [en]

Persistent Organic Pollutants (POPs) are a huge group of chemicals that have been linked to various adverse health effects in humans. Large epidemiological studies investigating gender differences in levels of POPs in the elderly are limited and the results from these are not always consistent. The present study was undertaken to examine the background levels of a broad range of POPs in human plasma samples among elderly men and women from Sweden and to assess the influence of gender. Levels of 23 POPs were determined in plasma samples collected during 2001-2004 from 1016 (50.2% women) 70year-old participants from the population-based Prospective Study of the Vasculature in Uppsala Seniors (PIVUS). Measurements were performed using high resolution gas chromatography with high resolution mass spectrometry (HRGC-HRMS) and the POPs studied were 16 polychlorinated biphenyls (PCBs), five organochlorine (OC) pesticides, one dioxin, and one brominated flame retardant. The concentrations of the selected POPs were found similar, or comparable, to other studies of non-occupationally exposed populations from Sweden and Europe. Differences in levels of POPs between men and women were assessed by using Wilcoxon rank-sum (Mann-Whitney) test. Significant (p<0.0001) gender differences in levels of specific POPs were observed and a number of POP concentrations were found to differ between men and women. More specifically, levels of HCB, OCDD, and PCB congeners #74, #105, and #118 were found to be higher in women, while the rest of the majority of POPs were higher in men.

National Category
Natural Sciences Chemical Sciences
Research subject
Chemistry
Identifiers
urn:nbn:se:oru:diva-23923 (URN)10.1016/j.envint.2012.01.011 (DOI)000304745900008 ()
Available from: 2012-07-05 Created: 2012-07-05 Last updated: 2017-12-07Bibliographically approved

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