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Improved cleanup of large lipid samples for electron capture gas chromatographic quantitation and gas chromatographic-mass spectrometric confirmation of organochlorine residues
Year:
1980
Authors :
Aharonson, Nadav
;
.
Veierov, Dan
;
.
Volume :
63
Co-Authors:
Veierov, D., Agric. Res. Organ., Volcani Cent., Bet Dagan, Israel
Aharonson, N., Agric. Res. Organ., Volcani Cent., Bet Dagan, Israel
Facilitators :
From page:
202
To page:
207
(
Total pages:
6
)
Abstract:
A new cleanup method for large lipid samples is described for the analysis of organochlorine traces. The method allows both electron capture gas chromatographic (GC) quantitation of sub-ppb levels and confirmation by GC-mass spectrometry. The lipid is extracted with concentrated sulfuric acid from a 2-5% solution of light petroleum ether. The method has been scaled up without increasing the petroleum volume by the alternate addition of lipids and sulfuric acid. Recovery studies were performed with 11 common organochlorine contaminants spiked in butterfat and in vegetable oils at the ppb level. The method is characterized by low lipid carryover of 0.02% by minimal use of solvent (about 2-3 mL/g lipid), and by its simplicity. A 50-200 g sample can be cleaned up in one day. Five μg of incurred p,p'-DDE has been cleaned up from a 50 g butterfat sample and purified by one TLC run. The eluted compound was analyzed by GC-MS and showed one peak (flame photometric detector) with a mass spectrum identical to authentic p,p'-DDE.
Note:
Related Files :
Chromatography, Gas
Dietary Fats
Gas Chromatography
Lipids
Pesticide Residues
vegetables
Show More
Related Content
More details
DOI :
Article number:
Affiliations:
Database:
Scopus
Publication Type:
article
;
.
Language:
English
Editors' remarks:
ID:
28491
Last updated date:
02/03/2022 17:27
Creation date:
17/04/2018 00:39
Scientific Publication
Improved cleanup of large lipid samples for electron capture gas chromatographic quantitation and gas chromatographic-mass spectrometric confirmation of organochlorine residues
63
Veierov, D., Agric. Res. Organ., Volcani Cent., Bet Dagan, Israel
Aharonson, N., Agric. Res. Organ., Volcani Cent., Bet Dagan, Israel
Improved cleanup of large lipid samples for electron capture gas chromatographic quantitation and gas chromatographic-mass spectrometric confirmation of organochlorine residues
A new cleanup method for large lipid samples is described for the analysis of organochlorine traces. The method allows both electron capture gas chromatographic (GC) quantitation of sub-ppb levels and confirmation by GC-mass spectrometry. The lipid is extracted with concentrated sulfuric acid from a 2-5% solution of light petroleum ether. The method has been scaled up without increasing the petroleum volume by the alternate addition of lipids and sulfuric acid. Recovery studies were performed with 11 common organochlorine contaminants spiked in butterfat and in vegetable oils at the ppb level. The method is characterized by low lipid carryover of 0.02% by minimal use of solvent (about 2-3 mL/g lipid), and by its simplicity. A 50-200 g sample can be cleaned up in one day. Five μg of incurred p,p'-DDE has been cleaned up from a 50 g butterfat sample and purified by one TLC run. The eluted compound was analyzed by GC-MS and showed one peak (flame photometric detector) with a mass spectrum identical to authentic p,p'-DDE.
Scientific Publication
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