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Gas chromatography/atmospheric pressure chemical ionization/mass spectrometry for the analysis of organochlorine pesticides and polychlorinated biphenyls in human serum
Örebro University, School of Science and Technology. (MTM Research Centre)ORCID iD: 0000-0002-8553-8824
Örebro University, School of Science and Technology. (MTM Research Centre)ORCID iD: 0000-0002-6330-789X
Waters Corporation, Manchester, United Kingdom.
Örebro University, School of Science and Technology. Department of Occupational and Environmental Medicine, Faculty of Medicine and Health, Örebro University, Örebro, Sweden. (MTM Research Centre)ORCID iD: 0000-0003-4128-8226
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2016 (English)In: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1453, 88-98 p.Article in journal (Refereed) Published
Resource type
Text
Abstract [en]

A method using a novel atmospheric pressure chemical ionization source for coupling gas chromatography (GC/APCI) to triple quadrupole mass spectrometry (MS/MS) for the determination of organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs) regulated by the Stockholm Convention is presented. One microliter injection of a six-point calibration curve of native PCBs and OCPs, ranging from 0.04 to 300 pg/μL, was performed. The relative standard deviation (RSD) of the relative response factors (RRFs) was less than 15% with a coefficient of determination (r2) >0.995. Meanwhile, two calibration solutions (CS), CS 2 (0.4 pg/μL) and CS 3 (4 pg/μL) were analyzed to study the repeatability calculated for both area and RRFs. The RSD for RRF ranged from 3.1 to 16% and 3.6 to 5.5% for CS 2 and CS 3, respectively. The limits of detection (LOD) determined by peak-to-peak signal-to-noise ratio (S/N) of 3 were compared between the GC/APCI/MS/MS and a GC coupled to high resolution mass spectrometry (GC/HRMS) system. GC/APCI/MS/MS resulted in lower LOD for most of the compounds, except for PCB#74, cis-chlordane and trans-chlordane. GC/APCI/MS/MS and GC/HRMS were also compared by performing analysis on 75 human serum samples together with eight QA/QC serum samples. The comparison between GC/APCI/MS/MS system and GC/HRMS system for 16 of the targeted compounds was carried out. No statistically significant difference was discovered. Due to increased sensitivity and user friendly operation under atmospheric pressure, GC/APCI/MS/MS is a powerful alternative technique that can easily meet the specification of GC/HRMS.

Place, publisher, year, edition, pages
Amsterdam, Netherlands: Elsevier, 2016. Vol. 1453, 88-98 p.
Keyword [en]
PCBs, OCPs, atmospheric pressure chemical ionization (APCI), triple quadrupole mass spectrometry (MS/MS), high resolution mass spectrometry (GC/HRMS), human serum
National Category
Chemical Sciences
Research subject
Analytical Chemistry; Environmental Chemistry; Enviromental Science
Identifiers
URN: urn:nbn:se:oru:diva-50854DOI: 10.1016/j.chroma.2016.05.030ISI: 000378182800010PubMedID: 27236485Scopus ID: 2-s2.0-84969722268OAI: oai:DiVA.org:oru-50854DiVA: diva2:937224
Note

Funding Agency:

China Scholarship Council (CSC) under the Grant CSC 201206400003

Available from: 2016-06-15 Created: 2016-06-14 Last updated: 2017-10-17Bibliographically approved
In thesis
1. Gas chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry methods for the determination of environmental contaminants
Open this publication in new window or tab >>Gas chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry methods for the determination of environmental contaminants
2016 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

The recent developments and improvements of instrumental methods for the analyses of the environmental contaminants, especially the persistent organic pollutants (POPs), have made it possible to detect and quantify these at very low concentrations in environmental and biotic matrices.

The main objective of this thesis is to demonstrate the capability of the atmospheric pressure chemical ionization technique (APCI), using gas chromatography coupled to tandem mass spectrometry for the determination of a wide range of environmental contaminants, including the POPs regulated by Stockholm Convention, such as polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs), polychlorinated biphenyls (PCBs), polybrominated diphenyl ethers (PBDEs), but also the derivates of PBDEs and novel brominated flame retardants (NBFRs).

The APCI was operated in charge transfer condition, preferably producing molecular ions. Multiple reaction monitoring (MRM) experiments were optimized by adjusting cone voltage, collision energy and dwell time. Optimization of source parameters, such as gas flows and temperatures was also performed. Low concentration standards were analyzed, achieving a visible chromatographic peak for 2 fg 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD) demonstrating the excellent sensitivity of the system. Adequate linearity and repeatability were observed for all the studied compounds. The performance of APCI methods was validated against the conventional methods using gas chromatography coupled to high resolution mass spectrometry for chlorinated compounds in a wide range of matrices including environmental, air, human and food matrices.

The GC-APCI-MS/MS method was successfully applied to a set of 75 human serum samples to study the circulating levels of POPs in epidemiologic studies. Moreover the method was utilized to establish temporal trends of POPs in osprey eggs samples collected during the past five decades.

Place, publisher, year, edition, pages
Örebro: Örebro university, 2016. 83 p.
Series
Örebro Studies in Chemistry, ISSN 1651-4270 ; 17
Keyword
PCDD/Fs, PCBs, OCPs, PBDEs, NBFRs, APCI, MS/MS, HRMS, human serum, osprey egg
National Category
Chemical Sciences Other Chemistry Topics
Research subject
Chemistry
Identifiers
urn:nbn:se:oru:diva-51727 (URN)978-91-7668-157-4 (ISBN)
Public defence
2016-09-30, Örebro universitet, Musikhögskolan, Hörsalen, Fakultetsgatan 1, Örebro, 10:15 (English)
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Available from: 2016-08-22 Created: 2016-08-22 Last updated: 2017-10-17Bibliographically approved

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