Simultaneous extraction and determination of HBCD isomers and TBBPA by ASE and LC-MSMS in fish

G. ten Dam, O. Pardo, W.A. Traag, M.K. van der Lee, R.J.B. Peters

Research output: Contribution to journalArticleAcademicpeer-review

43 Citations (Scopus)

Abstract

Since the EFSA enquired a call for data for TBBPA and HBCD in 2009, the analytical determination of these compounds in food became of regulatory interest. Therefore, a method for the simultaneous determination of TBBPA and the three major HBCD stereoisomers was developed. Conventional techniques like soxhlet, ASE, GPC, sulphuric acid digestion, and acidified silica SPE are generally used in sample pre-treatment while detection is mostly performed by LC–MSMS. A combined analysis of HBCD and TBBPA is problematic due to the hydroxyl groups in the TBBPA molecule. However, using a specific mesh-size sodium sulphate in ASE extraction and an acid silica column combined with a Sep-pack Plus silica cartridge for purification resulted in recoveries between 80% and 110% for all compounds. The accuracy and reproducibility determined using proficiency test samples were 104% and 4% for the sum of the HBCD isomers. Typical limits of detection were 0.01 ng/g product or 0.004 ng on column, while the linear dynamic range is between 0.01 ng and 10 ng on column. Levels of TBBPA and HBCD isomers were determined in eel samples. TBBPA was occasionally detected and only marginally above the quantification limit of 0.05 ng/g, whereas total amounts of HBCD were between 0.2 and 150 ng/g with a-HBCD being the dominant HBCD isomer.
Original languageEnglish
Pages (from-to)101-110
Number of pages10
JournalJournal of Chromatography. B, Analytical technologies in the biomedical and life sciences
Volume898
DOIs
Publication statusPublished - 2012

Fingerprint

Silicon Dioxide
Isomers
Fish
Fishes
Eels
Stereoisomerism
Acids
Hydroxyl Radical
Purification
Limit of Detection
Digestion
Recovery
Food
Molecules
sodium sulfate

Keywords

  • brominated flame retardants
  • enantiomer-specific accumulation
  • tandem mass-spectrometry
  • hexabromocyclododecane diastereoisomers
  • tetrabromobisphenol
  • biota

Cite this

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title = "Simultaneous extraction and determination of HBCD isomers and TBBPA by ASE and LC-MSMS in fish",
abstract = "Since the EFSA enquired a call for data for TBBPA and HBCD in 2009, the analytical determination of these compounds in food became of regulatory interest. Therefore, a method for the simultaneous determination of TBBPA and the three major HBCD stereoisomers was developed. Conventional techniques like soxhlet, ASE, GPC, sulphuric acid digestion, and acidified silica SPE are generally used in sample pre-treatment while detection is mostly performed by LC–MSMS. A combined analysis of HBCD and TBBPA is problematic due to the hydroxyl groups in the TBBPA molecule. However, using a specific mesh-size sodium sulphate in ASE extraction and an acid silica column combined with a Sep-pack Plus silica cartridge for purification resulted in recoveries between 80{\%} and 110{\%} for all compounds. The accuracy and reproducibility determined using proficiency test samples were 104{\%} and 4{\%} for the sum of the HBCD isomers. Typical limits of detection were 0.01 ng/g product or 0.004 ng on column, while the linear dynamic range is between 0.01 ng and 10 ng on column. Levels of TBBPA and HBCD isomers were determined in eel samples. TBBPA was occasionally detected and only marginally above the quantification limit of 0.05 ng/g, whereas total amounts of HBCD were between 0.2 and 150 ng/g with a-HBCD being the dominant HBCD isomer.",
keywords = "brominated flame retardants, enantiomer-specific accumulation, tandem mass-spectrometry, hexabromocyclododecane diastereoisomers, tetrabromobisphenol, biota",
author = "{ten Dam}, G. and O. Pardo and W.A. Traag and {van der Lee}, M.K. and R.J.B. Peters",
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language = "English",
volume = "898",
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}

Simultaneous extraction and determination of HBCD isomers and TBBPA by ASE and LC-MSMS in fish. / ten Dam, G.; Pardo, O.; Traag, W.A.; van der Lee, M.K.; Peters, R.J.B.

In: Journal of Chromatography. B, Analytical technologies in the biomedical and life sciences, Vol. 898, 2012, p. 101-110.

Research output: Contribution to journalArticleAcademicpeer-review

TY - JOUR

T1 - Simultaneous extraction and determination of HBCD isomers and TBBPA by ASE and LC-MSMS in fish

AU - ten Dam, G.

AU - Pardo, O.

AU - Traag, W.A.

AU - van der Lee, M.K.

AU - Peters, R.J.B.

PY - 2012

Y1 - 2012

N2 - Since the EFSA enquired a call for data for TBBPA and HBCD in 2009, the analytical determination of these compounds in food became of regulatory interest. Therefore, a method for the simultaneous determination of TBBPA and the three major HBCD stereoisomers was developed. Conventional techniques like soxhlet, ASE, GPC, sulphuric acid digestion, and acidified silica SPE are generally used in sample pre-treatment while detection is mostly performed by LC–MSMS. A combined analysis of HBCD and TBBPA is problematic due to the hydroxyl groups in the TBBPA molecule. However, using a specific mesh-size sodium sulphate in ASE extraction and an acid silica column combined with a Sep-pack Plus silica cartridge for purification resulted in recoveries between 80% and 110% for all compounds. The accuracy and reproducibility determined using proficiency test samples were 104% and 4% for the sum of the HBCD isomers. Typical limits of detection were 0.01 ng/g product or 0.004 ng on column, while the linear dynamic range is between 0.01 ng and 10 ng on column. Levels of TBBPA and HBCD isomers were determined in eel samples. TBBPA was occasionally detected and only marginally above the quantification limit of 0.05 ng/g, whereas total amounts of HBCD were between 0.2 and 150 ng/g with a-HBCD being the dominant HBCD isomer.

AB - Since the EFSA enquired a call for data for TBBPA and HBCD in 2009, the analytical determination of these compounds in food became of regulatory interest. Therefore, a method for the simultaneous determination of TBBPA and the three major HBCD stereoisomers was developed. Conventional techniques like soxhlet, ASE, GPC, sulphuric acid digestion, and acidified silica SPE are generally used in sample pre-treatment while detection is mostly performed by LC–MSMS. A combined analysis of HBCD and TBBPA is problematic due to the hydroxyl groups in the TBBPA molecule. However, using a specific mesh-size sodium sulphate in ASE extraction and an acid silica column combined with a Sep-pack Plus silica cartridge for purification resulted in recoveries between 80% and 110% for all compounds. The accuracy and reproducibility determined using proficiency test samples were 104% and 4% for the sum of the HBCD isomers. Typical limits of detection were 0.01 ng/g product or 0.004 ng on column, while the linear dynamic range is between 0.01 ng and 10 ng on column. Levels of TBBPA and HBCD isomers were determined in eel samples. TBBPA was occasionally detected and only marginally above the quantification limit of 0.05 ng/g, whereas total amounts of HBCD were between 0.2 and 150 ng/g with a-HBCD being the dominant HBCD isomer.

KW - brominated flame retardants

KW - enantiomer-specific accumulation

KW - tandem mass-spectrometry

KW - hexabromocyclododecane diastereoisomers

KW - tetrabromobisphenol

KW - biota

U2 - 10.1016/j.jchromb.2012.04.025

DO - 10.1016/j.jchromb.2012.04.025

M3 - Article

VL - 898

SP - 101

EP - 110

JO - Journal of Chromatography. B, Analytical technologies in the biomedical and life sciences

JF - Journal of Chromatography. B, Analytical technologies in the biomedical and life sciences

SN - 1570-0232

ER -