Simultaneous determination of dechloranes, polybrominated diphenyl ethers and novel brominated flame retardants in food and serum
A sensitive method for the simultaneous quantification of dechloranes, polybrominated diphenyl ethers (PBDEs) and novel brominated flame retardants (NBFRs) has been developed for gas chromatography (GC) coupled to tandem mass spectrometry operating in electron capture negative ionization (ECNI) mode...
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| Published in | Analytical and bioanalytical chemistry Vol. 409; no. 19; pp. 4507 - 4515 |
|---|---|
| Main Authors | , , , , , |
| Format | Journal Article |
| Language | English |
| Published |
Berlin/Heidelberg
Springer Berlin Heidelberg
01.07.2017
Springer Nature B.V |
| Subjects | |
| Online Access | Get full text |
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| Abstract | A sensitive method for the simultaneous quantification of dechloranes, polybrominated diphenyl ethers (PBDEs) and novel brominated flame retardants (NBFRs) has been developed for gas chromatography (GC) coupled to tandem mass spectrometry operating in electron capture negative ionization (ECNI) mode. The major advance has been achieved by combining selected ion monitoring (SIM) and multiple reaction monitoring (MRM) modes in well-defined time windows, to determine dechloranes, PBDEs and NBFRs at picogram per gram level in one single analysis in complex matrix biological samples. From the chromatographic point of view, efforts were devoted to study several injection modes using multimode inlet (MMI) in order to obtain low instrumental detection limits, necessary for trace compounds such as Dechlorane Plus (DP) isomers. Method performance was also evaluated: calibration curves were linear from 20 fg μL
−1
to 100 pg μL
−1
for the studied compounds, with method detection limits at levels of 50 fg g
−1
for DPs. Repeatability and reproducibility, expressed as relative standard deviation, were better than 5% even in solvent vent mode for the injection of standards. The application to a wide range of complex samples (including food, human and animal serum samples) indicated a sensitive and reliable way to quantify at the picogram per gram level 4 halogenated norbornenes (HNs), Dechlorane Plus (
anti
-DP and
syn
-DP) and 2 of their homologues (Dechlorane-602 and Dechlorane-603), 11 PBDE congeners (no. 28, 47, 49, 66, 85, 99, 100, 153, 154, 183 and 209) and 5 novel BFRs, i.e. decabromodiphenyl ethane (DBDPE), 1,2-bis(2,4,6-tribromophenoxy)ethane (BTBPE), hexabromobenzene (HBB), 2,3,4,5-tetrabromo-ethylhexyl-benzoate (TBB) and tetrabromophthalate (TBPH).
Graphical Abstract
GC-ECNI-MS/MS chromatograms showing the most sensitive transition for DPs when injecting 2 μL of a 16 fg/μL standard solution of s-DP and a-DP at three different source temperatures |
|---|---|
| AbstractList | A sensitive method for the simultaneous quantification of dechloranes, polybrominated diphenyl ethers (PBDEs) and novel brominated flame retardants (NBFRs) has been developed for gas chromatography (GC) coupled to tandem mass spectrometry operating in electron capture negative ionization (ECNI) mode. The major advance has been achieved by combining selected ion monitoring (SIM) and multiple reaction monitoring (MRM) modes in well-defined time windows, to determine dechloranes, PBDEs and NBFRs at picogram per gram level in one single analysis in complex matrix biological samples. From the chromatographic point of view, efforts were devoted to study several injection modes using multimode inlet (MMI) in order to obtain low instrumental detection limits, necessary for trace compounds such as Dechlorane Plus (DP) isomers. Method performance was also evaluated: calibration curves were linear from 20 fg μL⁻¹ to 100 pg μL⁻¹ for the studied compounds, with method detection limits at levels of 50 fg g⁻¹ for DPs. Repeatability and reproducibility, expressed as relative standard deviation, were better than 5% even in solvent vent mode for the injection of standards. The application to a wide range of complex samples (including food, human and animal serum samples) indicated a sensitive and reliable way to quantify at the picogram per gram level 4 halogenated norbornenes (HNs), Dechlorane Plus (anti-DP and syn-DP) and 2 of their homologues (Dechlorane-602 and Dechlorane-603), 11 PBDE congeners (no. 28, 47, 49, 66, 85, 99, 100, 153, 154, 183 and 209) and 5 novel BFRs, i.e. decabromodiphenyl ethane (DBDPE), 1,2-bis(2,4,6-tribromophenoxy)ethane (BTBPE), hexabromobenzene (HBB), 2,3,4,5-tetrabromo-ethylhexyl-benzoate (TBB) and tetrabromophthalate (TBPH). Graphical Abstract GC-ECNI-MS/MS chromatograms showing the most sensitive transition for DPs when injecting 2 μL of a 16 fg/μL standard solution of s-DP and a-DP at three different source temperatures A sensitive method for the simultaneous quantification of dechloranes, polybrominated diphenyl ethers (PBDEs) and novel brominated flame retardants (NBFRs) has been developed for gas chromatography (GC) coupled to tandem mass spectrometry operating in electron capture negative ionization (ECNI) mode. The major advance has been achieved by combining selected ion monitoring (SIM) and multiple reaction monitoring (MRM) modes in well-defined time windows, to determine dechloranes, PBDEs and NBFRs at picogram per gram level in one single analysis in complex matrix biological samples. From the chromatographic point of view, efforts were devoted to study several injection modes using multimode inlet (MMI) in order to obtain low instrumental detection limits, necessary for trace compounds such as Dechlorane Plus (DP) isomers. Method performance was also evaluated: calibration curves were linear from 20 fg μL−1 to 100 pg μL−1 for the studied compounds, with method detection limits at levels of 50 fg g−1 for DPs. Repeatability and reproducibility, expressed as relative standard deviation, were better than 5% even in solvent vent mode for the injection of standards. The application to a wide range of complex samples (including food, human and animal serum samples) indicated a sensitive and reliable way to quantify at the picogram per gram level 4 halogenated norbornenes (HNs), Dechlorane Plus (anti-DP and syn-DP) and 2 of their homologues (Dechlorane-602 and Dechlorane-603), 11 PBDE congeners (no. 28, 47, 49, 66, 85, 99, 100, 153, 154, 183 and 209) and 5 novel BFRs, i.e. decabromodiphenyl ethane (DBDPE), 1,2-bis(2,4,6-tribromophenoxy)ethane (BTBPE), hexabromobenzene (HBB), 2,3,4,5-tetrabromo-ethylhexyl-benzoate (TBB) and tetrabromophthalate (TBPH). A sensitive method for the simultaneous quantification of dechloranes, polybrominated diphenyl ethers (PBDEs) and novel brominated flame retardants (NBFRs) has been developed for gas chromatography (GC) coupled to tandem mass spectrometry operating in electron capture negative ionization (ECNI) mode. The major advance has been achieved by combining selected ion monitoring (SIM) and multiple reaction monitoring (MRM) modes in well-defined time windows, to determine dechloranes, PBDEs and NBFRs at picogram per gram level in one single analysis in complex matrix biological samples. From the chromatographic point of view, efforts were devoted to study several injection modes using multimode inlet (MMI) in order to obtain low instrumental detection limits, necessary for trace compounds such as Dechlorane Plus (DP) isomers. Method performance was also evaluated: calibration curves were linear from 20 fg μL −1 to 100 pg μL −1 for the studied compounds, with method detection limits at levels of 50 fg g −1 for DPs. Repeatability and reproducibility, expressed as relative standard deviation, were better than 5% even in solvent vent mode for the injection of standards. The application to a wide range of complex samples (including food, human and animal serum samples) indicated a sensitive and reliable way to quantify at the picogram per gram level 4 halogenated norbornenes (HNs), Dechlorane Plus ( anti -DP and syn -DP) and 2 of their homologues (Dechlorane-602 and Dechlorane-603), 11 PBDE congeners (no. 28, 47, 49, 66, 85, 99, 100, 153, 154, 183 and 209) and 5 novel BFRs, i.e. decabromodiphenyl ethane (DBDPE), 1,2-bis(2,4,6-tribromophenoxy)ethane (BTBPE), hexabromobenzene (HBB), 2,3,4,5-tetrabromo-ethylhexyl-benzoate (TBB) and tetrabromophthalate (TBPH). Graphical Abstract GC-ECNI-MS/MS chromatograms showing the most sensitive transition for DPs when injecting 2 μL of a 16 fg/μL standard solution of s-DP and a-DP at three different source temperatures A sensitive method for the simultaneous quantification of dechloranes, polybrominated diphenyl ethers (PBDEs) and novel brominated flame retardants (NBFRs) has been developed for gas chromatography (GC) coupled to tandem mass spectrometry operating in electron capture negative ionization (ECNI) mode. The major advance has been achieved by combining selected ion monitoring (SIM) and multiple reaction monitoring (MRM) modes in well-defined time windows, to determine dechloranes, PBDEs and NBFRs at picogram per gram level in one single analysis in complex matrix biological samples. From the chromatographic point of view, efforts were devoted to study several injection modes using multimode inlet (MMI) in order to obtain low instrumental detection limits, necessary for trace compounds such as Dechlorane Plus (DP) isomers. Method performance was also evaluated: calibration curves were linear from 20 fg μL-1 to 100 pg μL-1 for the studied compounds, with method detection limits at levels of 50 fg g-1 for DPs. Repeatability and reproducibility, expressed as relative standard deviation, were better than 5% even in solvent vent mode for the injection of standards. The application to a wide range of complex samples (including food, human and animal serum samples) indicated a sensitive and reliable way to quantify at the picogram per gram level 4 halogenated norbornenes (HNs), Dechlorane Plus (anti-DP and syn-DP) and 2 of their homologues (Dechlorane-602 and Dechlorane-603), 11 PBDE congeners (no. 28, 47, 49, 66, 85, 99, 100, 153, 154, 183 and 209) and 5 novel BFRs, i.e. decabromodiphenyl ethane (DBDPE), 1,2-bis(2,4,6-tribromophenoxy)ethane (BTBPE), hexabromobenzene (HBB), 2,3,4,5-tetrabromo-ethylhexyl-benzoate (TBB) and tetrabromophthalate (TBPH). Graphical Abstract GC-ECNI-MS/MS chromatograms showing the most sensitive transition for DPs when injecting 2 μL of a 16 fg/μL standard solution of s-DP and a-DP at three different source temperatures.A sensitive method for the simultaneous quantification of dechloranes, polybrominated diphenyl ethers (PBDEs) and novel brominated flame retardants (NBFRs) has been developed for gas chromatography (GC) coupled to tandem mass spectrometry operating in electron capture negative ionization (ECNI) mode. The major advance has been achieved by combining selected ion monitoring (SIM) and multiple reaction monitoring (MRM) modes in well-defined time windows, to determine dechloranes, PBDEs and NBFRs at picogram per gram level in one single analysis in complex matrix biological samples. From the chromatographic point of view, efforts were devoted to study several injection modes using multimode inlet (MMI) in order to obtain low instrumental detection limits, necessary for trace compounds such as Dechlorane Plus (DP) isomers. Method performance was also evaluated: calibration curves were linear from 20 fg μL-1 to 100 pg μL-1 for the studied compounds, with method detection limits at levels of 50 fg g-1 for DPs. Repeatability and reproducibility, expressed as relative standard deviation, were better than 5% even in solvent vent mode for the injection of standards. The application to a wide range of complex samples (including food, human and animal serum samples) indicated a sensitive and reliable way to quantify at the picogram per gram level 4 halogenated norbornenes (HNs), Dechlorane Plus (anti-DP and syn-DP) and 2 of their homologues (Dechlorane-602 and Dechlorane-603), 11 PBDE congeners (no. 28, 47, 49, 66, 85, 99, 100, 153, 154, 183 and 209) and 5 novel BFRs, i.e. decabromodiphenyl ethane (DBDPE), 1,2-bis(2,4,6-tribromophenoxy)ethane (BTBPE), hexabromobenzene (HBB), 2,3,4,5-tetrabromo-ethylhexyl-benzoate (TBB) and tetrabromophthalate (TBPH). Graphical Abstract GC-ECNI-MS/MS chromatograms showing the most sensitive transition for DPs when injecting 2 μL of a 16 fg/μL standard solution of s-DP and a-DP at three different source temperatures. A sensitive method for the simultaneous quantification of dechloranes, polybrominated diphenyl ethers (PBDEs) and novel brominated flame retardants (NBFRs) has been developed for gas chromatography (GC) coupled to tandem mass spectrometry operating in electron capture negative ionization (ECNI) mode. The major advance has been achieved by combining selected ion monitoring (SIM) and multiple reaction monitoring (MRM) modes in well-defined time windows, to determine dechloranes, PBDEs and NBFRs at picogram per gram level in one single analysis in complex matrix biological samples. From the chromatographic point of view, efforts were devoted to study several injection modes using multimode inlet (MMI) in order to obtain low instrumental detection limits, necessary for trace compounds such as Dechlorane Plus (DP) isomers. Method performance was also evaluated: calibration curves were linear from 20 fg μL to 100 pg μL for the studied compounds, with method detection limits at levels of 50 fg g for DPs. Repeatability and reproducibility, expressed as relative standard deviation, were better than 5% even in solvent vent mode for the injection of standards. The application to a wide range of complex samples (including food, human and animal serum samples) indicated a sensitive and reliable way to quantify at the picogram per gram level 4 halogenated norbornenes (HNs), Dechlorane Plus (anti-DP and syn-DP) and 2 of their homologues (Dechlorane-602 and Dechlorane-603), 11 PBDE congeners (no. 28, 47, 49, 66, 85, 99, 100, 153, 154, 183 and 209) and 5 novel BFRs, i.e. decabromodiphenyl ethane (DBDPE), 1,2-bis(2,4,6-tribromophenoxy)ethane (BTBPE), hexabromobenzene (HBB), 2,3,4,5-tetrabromo-ethylhexyl-benzoate (TBB) and tetrabromophthalate (TBPH). Graphical Abstract GC-ECNI-MS/MS chromatograms showing the most sensitive transition for DPs when injecting 2 μL of a 16 fg/μL standard solution of s-DP and a-DP at three different source temperatures. |
| Author | Covaci, Adrian Poma, Giulia Malarvannan, Govindan Sales, Carlos Portolés, Tania Beltrán, Joaquin |
| Author_xml | – sequence: 1 givenname: Carlos orcidid: 0000-0001-6337-063X surname: Sales fullname: Sales, Carlos email: casales@uji.es organization: Research Institute for Pesticides and Water, University Jaume I – sequence: 2 givenname: Giulia surname: Poma fullname: Poma, Giulia organization: Toxicological Centre, Department of Pharmaceutical Sciences, University of Antwerp – sequence: 3 givenname: Govindan surname: Malarvannan fullname: Malarvannan, Govindan organization: Toxicological Centre, Department of Pharmaceutical Sciences, University of Antwerp – sequence: 4 givenname: Tania surname: Portolés fullname: Portolés, Tania organization: Research Institute for Pesticides and Water, University Jaume I – sequence: 5 givenname: Joaquin surname: Beltrán fullname: Beltrán, Joaquin organization: Research Institute for Pesticides and Water, University Jaume I – sequence: 6 givenname: Adrian surname: Covaci fullname: Covaci, Adrian email: adrian.covaci@uantwerpen.be organization: Toxicological Centre, Department of Pharmaceutical Sciences, University of Antwerp |
| BackLink | https://www.ncbi.nlm.nih.gov/pubmed/28593372$$D View this record in MEDLINE/PubMed |
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| Copyright | Springer-Verlag Berlin Heidelberg 2017 Analytical and Bioanalytical Chemistry is a copyright of Springer, (2017). All Rights Reserved. |
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| Keywords | Gas chromatography Biological matrices Dechloranes Brominated flame retardants Chemical ionization Large volume injection |
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| PublicationTitle | Analytical and bioanalytical chemistry |
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| References_xml | – volume: 87 start-page: 9892 year: 2015 end-page: 9899 ident: CR10 article-title: Novel analytical approach for brominated flame retardants based on the use of gas chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry with emphasis in highly brominated congeners publication-title: Anal Chem doi: 10.1021/acs.analchem.5b02378 – volume: 46 start-page: 583 year: 2002 end-page: 624 ident: CR1 article-title: An overview of brominated flame retardants in the environment publication-title: Chemosphere doi: 10.1016/S0045-6535(01)00225-9 – volume: 65 start-page: 147 year: 2014 end-page: 158 ident: CR3 article-title: Levels and trends of PBDEs and HBCDs in the global environment: status at the end of 2012 publication-title: Environ Int doi: 10.1016/j.envint.2014.01.006 – volume: 30 start-page: 2545 year: 2016 end-page: 2554 ident: CR16 article-title: Measurement of emerging dechloranes in human serum using modulated gas chromatography coupled to 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10.1016/S0160-4120(03)00123-5 – volume: 49 start-page: 31 year: 2012 end-page: 37 ident: CR19 article-title: Dechlorane plus in serum from e-waste recycling workers: influence of gender and potential isomer-specific metabolism publication-title: Environ Int doi: 10.1016/j.envint.2012.08.011 – volume: 14 start-page: 1 year: 2015 end-page: 11 ident: CR7 article-title: Polybrominated diphenyl ether serum concentrations in a Californian population of children, their parents, and older adults: an exposure assessment study publication-title: Environ Health doi: 10.1186/s12940-015-0002-2 – volume: 65 start-page: 168 year: 2016 end-page: 176 ident: CR25 article-title: Determination of halogenated flame retardants in food: optimization and validation of a method based on a two-step clean-up and gas chromatography-mass spectrometry publication-title: Food Control doi: 10.1016/j.foodcont.2016.01.027 – volume: 66 start-page: 11 year: 2014 end-page: 17 ident: CR21 article-title: Hexachloronorbornene-based flame retardants in humans: levels in maternal serum and milk publication-title: Environ Int doi: 10.1016/j.envint.2014.01.010 – volume: 88 start-page: 11406 year: 2016 end-page: 11411 ident: CR11 article-title: Determination of halogenated flame retardants using gas chromatography with atmospheric pressure chemical ionization (APCI) and a high-resolution quadrupole time-of-flight mass spectrometer (HRqTOFMS) publication-title: Anal Chem doi: 10.1021/acs.analchem.6b01550 – volume: 74 start-page: 54 year: 2015 end-page: 59 ident: CR23 article-title: Comparing human exposure to emerging and legacy fl ame retardants from the indoor environment and diet with concentrations measured in serum publication-title: Environ Int doi: 10.1016/j.envint.2014.10.003 – volume: 37 start-page: 532 year: 2011 end-page: 556 ident: CR5 article-title: Novel brominated flame retardants: a review of their analysis, environmental fate and behaviour publication-title: Environ Int doi: 10.1016/j.envint.2010.11.007 – volume: 47 start-page: 12441 year: 2013 end-page: 12449 ident: CR26 article-title: Dynamics of organohalogenated contaminants in human serum from obese individuals during one year of weight loss treatment publication-title: Environ Sci Technol doi: 10.1021/es400657t – volume: 32 start-page: 1242 year: 2013 end-page: 1247 ident: CR20 article-title: Concentrations and trends of halogenated flame retardants in the pooled serum of residents of Laizhou Bay, China publication-title: Environ Toxicol Chem doi: 10.1002/etc.2172 – volume: 46 start-page: 13056 issue: 24 year: 2012 end-page: 13066 ident: CR6 article-title: After the PBDE phase-out: a broad suite of flame retardants in repeat house dust samples from California publication-title: Environ Sci Technol doi: 10.1021/es303879n – volume: 45 start-page: 5088 year: 2011 end-page: 5098 ident: CR15 article-title: Dechlorane plus and related compounds in the environment: a review publication-title: Environ Sci Technol doi: 10.1021/es2003028 – volume: 1310 start-page: 126 year: 2013 end-page: 132 ident: CR22 article-title: Determination of emerging halogenated flame retardants and polybrominated diphenyl ethers in serum by gas chromatography mass spectrometry publication-title: J Chromatogr A doi: 10.1016/j.chroma.2013.08.067 – volume: 44 start-page: 760 year: 2010 end-page: 766 ident: CR13 article-title: Identification and screening analysis of halogenated norbornene flame retardants in the Laurentian Great Lakes: Dechloranes 602, 603, and 604 publication-title: Environ Sci Technol doi: 10.1021/es902482b – volume: 43 start-page: 9453 year: 2009 end-page: 9457 ident: CR18 article-title: Determination of dechlorane plus in serum from electronics dismantling workers in South China publication-title: Environ Sci Technol doi: 10.1021/es901672m – volume: 1248 start-page: 154 year: 2012 end-page: 160 ident: CR28 article-title: Analytical method for the determination of halogenated norbornene flame 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| Title | Simultaneous determination of dechloranes, polybrominated diphenyl ethers and novel brominated flame retardants in food and serum |
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