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Multivariate optimization of high-pressure supercritical carbon dioxide extraction technique for analysis of selected pesticides in green coffee beans

Gemechu, Tura ; Tolcha, Teshome ; Al-Hamimi, Said LU ; Turner, Charlotta LU orcid ; Chandravanshi, Bhagwan Singh and Megersa, Negussie LU (2026) In Bulletin of the Chemical Society of Ethiopia 40(1). p.183-197
Abstract

Residues of pesticides require efficient and selective sample preparation, due to their existence in trace levels and the complex nature of food matrices. The objective of this study was to use a multivariate experimental design for the determination of multi-residue pesticides in the green coffee beans utilizing supercritical carbon dioxide (sc-CO2) as extraction solvent. In this study, an extraction method based on sc-CO2 as a solvent, at high pressure using Al2O3 as a masking agent for caffeine removal, was developed for the determination of pesticide residues in green coffee beans. A Box-Behnken experimental design was utilized to optimize extraction parameters, including pressure (200-800 bar), temperature (40-70 ℃), and volumes of... (More)

Residues of pesticides require efficient and selective sample preparation, due to their existence in trace levels and the complex nature of food matrices. The objective of this study was to use a multivariate experimental design for the determination of multi-residue pesticides in the green coffee beans utilizing supercritical carbon dioxide (sc-CO2) as extraction solvent. In this study, an extraction method based on sc-CO2 as a solvent, at high pressure using Al2O3 as a masking agent for caffeine removal, was developed for the determination of pesticide residues in green coffee beans. A Box-Behnken experimental design was utilized to optimize extraction parameters, including pressure (200-800 bar), temperature (40-70 ℃), and volumes of sc-CO2 (10-40 mL). The optimum extraction conditions were found to be 588 bar, 46 °C, and 40 mL. The method's performance was evaluated by extracting 5 µg g-1 spiked green coffee bean samples, resulting in good linearity (R2 ≥ 0.995); repeatability (3.7-10.3%), and reproducibility (1.6-8.4%). Limit of detection (LODs), Limit of quantification (LOQs), and recoveries were in the ranges 0.02-0.05 µg g-1, 0.08-0.13 µg g-1, and 86-97%, respectively. The developed method could be used as an alternative method for the determination of α-hexachlorohexane (α-HCH), lindane, β-hexachlorohexane (β-HCH), and malathion in green coffee beans.

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author
; ; ; ; and
organization
publishing date
type
Contribution to journal
publication status
published
subject
keywords
GC-MS, Green coffee bean, Multivariate optimization, Pesticide residues, sc-CO2
in
Bulletin of the Chemical Society of Ethiopia
volume
40
issue
1
pages
15 pages
publisher
Chemical Society of Ethiopia
external identifiers
  • scopus:105038310026
ISSN
1011-3924
DOI
10.4314/bcse.v40i1.15
language
English
LU publication?
yes
id
8f688cdd-b288-4f5e-af1c-b9a05c2cd9fe
date added to LUP
2026-08-19 11:21:48
date last changed
2026-08-19 11:22:40
@article{8f688cdd-b288-4f5e-af1c-b9a05c2cd9fe,
  abstract     = {{<p>Residues of pesticides require efficient and selective sample preparation, due to their existence in trace levels and the complex nature of food matrices. The objective of this study was to use a multivariate experimental design for the determination of multi-residue pesticides in the green coffee beans utilizing supercritical carbon dioxide (sc-CO2) as extraction solvent. In this study, an extraction method based on sc-CO2 as a solvent, at high pressure using Al2O3 as a masking agent for caffeine removal, was developed for the determination of pesticide residues in green coffee beans. A Box-Behnken experimental design was utilized to optimize extraction parameters, including pressure (200-800 bar), temperature (40-70 ℃), and volumes of sc-CO2 (10-40 mL). The optimum extraction conditions were found to be 588 bar, 46 °C, and 40 mL. The method's performance was evaluated by extracting 5 µg g<sup>-1</sup> spiked green coffee bean samples, resulting in good linearity (R<sup>2</sup> ≥ 0.995); repeatability (3.7-10.3%), and reproducibility (1.6-8.4%). Limit of detection (LODs), Limit of quantification (LOQs), and recoveries were in the ranges 0.02-0.05 µg g<sup>-1</sup>, 0.08-0.13 µg g<sup>-1</sup>, and 86-97%, respectively. The developed method could be used as an alternative method for the determination of α-hexachlorohexane (α-HCH), lindane, β-hexachlorohexane (β-HCH), and malathion in green coffee beans.</p>}},
  author       = {{Gemechu, Tura and Tolcha, Teshome and Al-Hamimi, Said and Turner, Charlotta and Chandravanshi, Bhagwan Singh and Megersa, Negussie}},
  issn         = {{1011-3924}},
  keywords     = {{GC-MS; Green coffee bean; Multivariate optimization; Pesticide residues; sc-CO2}},
  language     = {{eng}},
  number       = {{1}},
  pages        = {{183--197}},
  publisher    = {{Chemical Society of Ethiopia}},
  series       = {{Bulletin of the Chemical Society of Ethiopia}},
  title        = {{Multivariate optimization of high-pressure supercritical carbon dioxide extraction technique for analysis of selected pesticides in green coffee beans}},
  url          = {{http://dx.doi.org/10.4314/bcse.v40i1.15}},
  doi          = {{10.4314/bcse.v40i1.15}},
  volume       = {{40}},
  year         = {{2026}},
}