Qualitative screening and quantitative determination of pesticides and contaminants in animal feed using comprehensive two-dimensional gas chomatography with time-of-flight mass spectrometry

M.K. van der Lee, G. van der Weg, W.A. Traag, J.G.J. Mol

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Abstract

A method has been developed for the target analysis of over 100 pesticides and contaminants in a complex feed matrix. The method is based on extraction with ethyl acetate, cleanup by gel permeation chromatography (GPC) and dispersive solid-phase extraction (SPE) with primary secondary amine phase (PSA), and analysis by comprehensive two-dimensional gas chromatography with full scan time-of-flight mass spectrometric detection (GC × GC¿TOF-MS). Parameters studied during method development included a dispersive SPE cleanup step after GPC, large volume injection into the GC system and the GC × GC separation. Qualitative and quantitative performance of the GC × GC system was evaluated by analyzing spiked extracts in the range equivalent to 1¿100 ¿g/kg in feed. At levels of 50 ¿g/kg and higher, all compounds targeted for could be identified fully automatically by the software based on their mass spectra. At lower levels the hit rate decreased with the concentration. System linearity was excellent in solvent and only slightly affected by matrix (correlation coefficients r ¿ 0.995 for 90% of the compounds). Limits of quantification were in the 1¿20 ¿g/kg range for most compounds. The overall method was validated for 106 compounds at the 10 and 100 ¿g/kg level. Recoveries between 70% and 110% and RSDs below 20% were obtained for the majority of the compounds.
Original languageEnglish
Pages (from-to)325-339
Number of pages15
JournalJournal of Chromatography. A, Including electrophoresis and other separation methods
Volume1186
Issue number1-2
DOIs
Publication statusPublished - 2008

Fingerprint

Pesticides
Mass spectrometry
Mass Spectrometry
Screening
Animals
Gases
Gel permeation chromatography
Impurities
Solid Phase Extraction
Gel Chromatography
Gas chromatography
Amines
Gas Chromatography
Recovery
Software
Injections

Keywords

  • gc x gc
  • fish feed
  • organochlorine pesticides
  • extraction
  • residues
  • pressure
  • volumes
  • dioxins
  • fruit
  • pcbs

Cite this

@article{3791810c298c4e008304c0c33f7c345a,
title = "Qualitative screening and quantitative determination of pesticides and contaminants in animal feed using comprehensive two-dimensional gas chomatography with time-of-flight mass spectrometry",
abstract = "A method has been developed for the target analysis of over 100 pesticides and contaminants in a complex feed matrix. The method is based on extraction with ethyl acetate, cleanup by gel permeation chromatography (GPC) and dispersive solid-phase extraction (SPE) with primary secondary amine phase (PSA), and analysis by comprehensive two-dimensional gas chromatography with full scan time-of-flight mass spectrometric detection (GC × GC¿TOF-MS). Parameters studied during method development included a dispersive SPE cleanup step after GPC, large volume injection into the GC system and the GC × GC separation. Qualitative and quantitative performance of the GC × GC system was evaluated by analyzing spiked extracts in the range equivalent to 1¿100 ¿g/kg in feed. At levels of 50 ¿g/kg and higher, all compounds targeted for could be identified fully automatically by the software based on their mass spectra. At lower levels the hit rate decreased with the concentration. System linearity was excellent in solvent and only slightly affected by matrix (correlation coefficients r ¿ 0.995 for 90{\%} of the compounds). Limits of quantification were in the 1¿20 ¿g/kg range for most compounds. The overall method was validated for 106 compounds at the 10 and 100 ¿g/kg level. Recoveries between 70{\%} and 110{\%} and RSDs below 20{\%} were obtained for the majority of the compounds.",
keywords = "gc x gc, fish feed, organochlorine pesticides, extraction, residues, pressure, volumes, dioxins, fruit, pcbs",
author = "{van der Lee}, M.K. and {van der Weg}, G. and W.A. Traag and J.G.J. Mol",
year = "2008",
doi = "10.1016/j.chroma.2007.11.043",
language = "English",
volume = "1186",
pages = "325--339",
journal = "Journal of Chromatography. A, Including electrophoresis and other separation methods",
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TY - JOUR

T1 - Qualitative screening and quantitative determination of pesticides and contaminants in animal feed using comprehensive two-dimensional gas chomatography with time-of-flight mass spectrometry

AU - van der Lee, M.K.

AU - van der Weg, G.

AU - Traag, W.A.

AU - Mol, J.G.J.

PY - 2008

Y1 - 2008

N2 - A method has been developed for the target analysis of over 100 pesticides and contaminants in a complex feed matrix. The method is based on extraction with ethyl acetate, cleanup by gel permeation chromatography (GPC) and dispersive solid-phase extraction (SPE) with primary secondary amine phase (PSA), and analysis by comprehensive two-dimensional gas chromatography with full scan time-of-flight mass spectrometric detection (GC × GC¿TOF-MS). Parameters studied during method development included a dispersive SPE cleanup step after GPC, large volume injection into the GC system and the GC × GC separation. Qualitative and quantitative performance of the GC × GC system was evaluated by analyzing spiked extracts in the range equivalent to 1¿100 ¿g/kg in feed. At levels of 50 ¿g/kg and higher, all compounds targeted for could be identified fully automatically by the software based on their mass spectra. At lower levels the hit rate decreased with the concentration. System linearity was excellent in solvent and only slightly affected by matrix (correlation coefficients r ¿ 0.995 for 90% of the compounds). Limits of quantification were in the 1¿20 ¿g/kg range for most compounds. The overall method was validated for 106 compounds at the 10 and 100 ¿g/kg level. Recoveries between 70% and 110% and RSDs below 20% were obtained for the majority of the compounds.

AB - A method has been developed for the target analysis of over 100 pesticides and contaminants in a complex feed matrix. The method is based on extraction with ethyl acetate, cleanup by gel permeation chromatography (GPC) and dispersive solid-phase extraction (SPE) with primary secondary amine phase (PSA), and analysis by comprehensive two-dimensional gas chromatography with full scan time-of-flight mass spectrometric detection (GC × GC¿TOF-MS). Parameters studied during method development included a dispersive SPE cleanup step after GPC, large volume injection into the GC system and the GC × GC separation. Qualitative and quantitative performance of the GC × GC system was evaluated by analyzing spiked extracts in the range equivalent to 1¿100 ¿g/kg in feed. At levels of 50 ¿g/kg and higher, all compounds targeted for could be identified fully automatically by the software based on their mass spectra. At lower levels the hit rate decreased with the concentration. System linearity was excellent in solvent and only slightly affected by matrix (correlation coefficients r ¿ 0.995 for 90% of the compounds). Limits of quantification were in the 1¿20 ¿g/kg range for most compounds. The overall method was validated for 106 compounds at the 10 and 100 ¿g/kg level. Recoveries between 70% and 110% and RSDs below 20% were obtained for the majority of the compounds.

KW - gc x gc

KW - fish feed

KW - organochlorine pesticides

KW - extraction

KW - residues

KW - pressure

KW - volumes

KW - dioxins

KW - fruit

KW - pcbs

U2 - 10.1016/j.chroma.2007.11.043

DO - 10.1016/j.chroma.2007.11.043

M3 - Article

VL - 1186

SP - 325

EP - 339

JO - Journal of Chromatography. A, Including electrophoresis and other separation methods

JF - Journal of Chromatography. A, Including electrophoresis and other separation methods

SN - 0021-9673

IS - 1-2

ER -