Rapid analytical method for the determination of pesticide residues in sunflower seeds based on focused microwave-assisted Soxhlet extraction prior to gas chromatography-tandem mass spectrometry

R. C. Prados-Rosales, J. L. Luque García, M. D. Luque De Castro

Research output: Contribution to journalArticle

44 Citations (Scopus)

Abstract

A rapid analytical method for determination of organochlorine pesticide residues in sunflower seeds based on focused microwave-assisted Soxhlet extraction has been developed. The main factors affecting the extraction efficiency - namely microwave power, irradiation time, volume of extractant and number of cycles - were optimized by a two-level factorial fractional design. After extraction, a liquid-liquid extraction and a clean-up step including the use of Florisil macrocolumns were required prior to injection of the extracts into the chromatograph in order to isolate the pesticide residues from the lipid fraction of the original extract. The MS-MS ion preparation mode was selected due to the high sensitivity and selectivity it provides. Seed samples were used collected near a crop subjected to aerial pesticide application. Residues of hexachlorocyclohexane isomers and endosulfan were found in the seeds although they were not subjected to pesticide application, thus showing the spray-drift contamination. The validation of the proposed approach was carried out by comparison with the ISO 659-1988 reference extraction method obtaining similar, or even better efficiencies by the proposed approach.

Original languageEnglish (US)
Pages (from-to)121-129
Number of pages9
JournalJournal of Chromatography A
Volume993
Issue number1-2
DOIs
StatePublished - Apr 18 2003
Externally publishedYes

Fingerprint

Pesticide Residues
Helianthus
Microwaves
Tandem Mass Spectrometry
Gas chromatography
Gas Chromatography-Mass Spectrometry
Mass spectrometry
Seed
Seeds
Pesticides
Endosulfan
Lindane
Liquid-Liquid Extraction
Ions
Lipids
Liquids
Injections
Isomers
Crops
Contamination

Keywords

  • Endosulfan
  • Extraction methods
  • Factorial design
  • Focused microwave-assisted Soxhlet extraction
  • Hexachlorocyclohexanes
  • Organochlorine compounds
  • Pesticides
  • Plant materials

ASJC Scopus subject areas

  • Analytical Chemistry

Cite this

Rapid analytical method for the determination of pesticide residues in sunflower seeds based on focused microwave-assisted Soxhlet extraction prior to gas chromatography-tandem mass spectrometry. / Prados-Rosales, R. C.; Luque García, J. L.; Luque De Castro, M. D.

In: Journal of Chromatography A, Vol. 993, No. 1-2, 18.04.2003, p. 121-129.

Research output: Contribution to journalArticle

@article{21565e338ce948aaa90d41435b1f68e1,
title = "Rapid analytical method for the determination of pesticide residues in sunflower seeds based on focused microwave-assisted Soxhlet extraction prior to gas chromatography-tandem mass spectrometry",
abstract = "A rapid analytical method for determination of organochlorine pesticide residues in sunflower seeds based on focused microwave-assisted Soxhlet extraction has been developed. The main factors affecting the extraction efficiency - namely microwave power, irradiation time, volume of extractant and number of cycles - were optimized by a two-level factorial fractional design. After extraction, a liquid-liquid extraction and a clean-up step including the use of Florisil macrocolumns were required prior to injection of the extracts into the chromatograph in order to isolate the pesticide residues from the lipid fraction of the original extract. The MS-MS ion preparation mode was selected due to the high sensitivity and selectivity it provides. Seed samples were used collected near a crop subjected to aerial pesticide application. Residues of hexachlorocyclohexane isomers and endosulfan were found in the seeds although they were not subjected to pesticide application, thus showing the spray-drift contamination. The validation of the proposed approach was carried out by comparison with the ISO 659-1988 reference extraction method obtaining similar, or even better efficiencies by the proposed approach.",
keywords = "Endosulfan, Extraction methods, Factorial design, Focused microwave-assisted Soxhlet extraction, Hexachlorocyclohexanes, Organochlorine compounds, Pesticides, Plant materials",
author = "Prados-Rosales, {R. C.} and {Luque Garc{\'i}a}, {J. L.} and {Luque De Castro}, {M. D.}",
year = "2003",
month = "4",
day = "18",
doi = "10.1016/S0021-9673(03)00396-0",
language = "English (US)",
volume = "993",
pages = "121--129",
journal = "Journal of Chromatography",
issn = "0021-9673",
publisher = "Elsevier",
number = "1-2",

}

TY - JOUR

T1 - Rapid analytical method for the determination of pesticide residues in sunflower seeds based on focused microwave-assisted Soxhlet extraction prior to gas chromatography-tandem mass spectrometry

AU - Prados-Rosales, R. C.

AU - Luque García, J. L.

AU - Luque De Castro, M. D.

PY - 2003/4/18

Y1 - 2003/4/18

N2 - A rapid analytical method for determination of organochlorine pesticide residues in sunflower seeds based on focused microwave-assisted Soxhlet extraction has been developed. The main factors affecting the extraction efficiency - namely microwave power, irradiation time, volume of extractant and number of cycles - were optimized by a two-level factorial fractional design. After extraction, a liquid-liquid extraction and a clean-up step including the use of Florisil macrocolumns were required prior to injection of the extracts into the chromatograph in order to isolate the pesticide residues from the lipid fraction of the original extract. The MS-MS ion preparation mode was selected due to the high sensitivity and selectivity it provides. Seed samples were used collected near a crop subjected to aerial pesticide application. Residues of hexachlorocyclohexane isomers and endosulfan were found in the seeds although they were not subjected to pesticide application, thus showing the spray-drift contamination. The validation of the proposed approach was carried out by comparison with the ISO 659-1988 reference extraction method obtaining similar, or even better efficiencies by the proposed approach.

AB - A rapid analytical method for determination of organochlorine pesticide residues in sunflower seeds based on focused microwave-assisted Soxhlet extraction has been developed. The main factors affecting the extraction efficiency - namely microwave power, irradiation time, volume of extractant and number of cycles - were optimized by a two-level factorial fractional design. After extraction, a liquid-liquid extraction and a clean-up step including the use of Florisil macrocolumns were required prior to injection of the extracts into the chromatograph in order to isolate the pesticide residues from the lipid fraction of the original extract. The MS-MS ion preparation mode was selected due to the high sensitivity and selectivity it provides. Seed samples were used collected near a crop subjected to aerial pesticide application. Residues of hexachlorocyclohexane isomers and endosulfan were found in the seeds although they were not subjected to pesticide application, thus showing the spray-drift contamination. The validation of the proposed approach was carried out by comparison with the ISO 659-1988 reference extraction method obtaining similar, or even better efficiencies by the proposed approach.

KW - Endosulfan

KW - Extraction methods

KW - Factorial design

KW - Focused microwave-assisted Soxhlet extraction

KW - Hexachlorocyclohexanes

KW - Organochlorine compounds

KW - Pesticides

KW - Plant materials

UR - http://www.scopus.com/inward/record.url?scp=0037453450&partnerID=8YFLogxK

UR - http://www.scopus.com/inward/citedby.url?scp=0037453450&partnerID=8YFLogxK

U2 - 10.1016/S0021-9673(03)00396-0

DO - 10.1016/S0021-9673(03)00396-0

M3 - Article

C2 - 12735444

AN - SCOPUS:0037453450

VL - 993

SP - 121

EP - 129

JO - Journal of Chromatography

JF - Journal of Chromatography

SN - 0021-9673

IS - 1-2

ER -