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A rapid method for analysis of PFAS including structural PFOS isomers in human serum using 96-well plate column-switching UPLC-S/MS
Örebro University, School of Science and Technology.ORCID iD: 0000-0001-5752-4196
Örebro University, School of Science and Technology.
Örebro University, School of Science and Technology.ORCID iD: 0000-0002-4959-2807
2Occupational and Environmental Medicine, Uppsala University, Uppsala, Sweden.
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(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 [en]
human blood, perfluoroalkylated substances, structural isomers, perfluorooctane sulfonamide, sample preparation, column-switch, pfos, pfoa
National Category
Chemical Sciences
Research subject
Chemistry
Identifiers
URN: urn:nbn:se:oru:diva-30109OAI: oai:DiVA.org:oru-30109DiVA, id: diva2:638784
Available from: 2013-08-02 Created: 2013-08-02 Last updated: 2017-10-17Bibliographically approved
In thesis
1. Development and application of high-throughput methods for analysis of persistent organic pollutants in human blood
Open this publication in new window or tab >>Development and application of high-throughput methods for analysis of persistent organic pollutants in human blood
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
Human blood, POPs, Perfluoroalkylated substances, Structural isomers, Sample preparation, Column-switch, Mass spectrometry
National Category
Chemical Sciences
Research subject
Chemistry
Identifiers
urn:nbn:se:oru:diva-28456 (URN)978-91-7668-936-3 (ISBN)
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

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Salihovic, SamiraKärrman, AnnaLindström, Gunillavan Bavel, Bert

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