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An efficient extraction and clean‐up procedure for pesticide determination in olive oil
Author(s) -
Sobhanzadeh Elham,
Bakar Nor Kartini Abu,
Abas Mhd Radzi Bin,
Nemati Keivan
Publication year - 2011
Publication title -
european journal of lipid science and technology
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.614
H-Index - 94
eISSN - 1438-9312
pISSN - 1438-7697
DOI - 10.1002/ejlt.201000384
Subject(s) - chromatography , chemistry , sorbent , extraction (chemistry) , sonication , solid phase extraction , detection limit , solvent , pesticide residue , matrix (chemical analysis) , clean up , dispersant , adsorption , pesticide , dispersion (optics) , organic chemistry , optics , agronomy , biology , physics
This work reports a simple, rapid, and effective extraction method based on liquid–liquid extraction (LLE) followed by matrix solid‐phase dispersion‐sonication for detection, identification and quantification of multiclass pesticides in virgin olive oil using liquid chromatography mass spectrometry (LC‐QTOF‐MS). LLE to extract pesticide residues in virgin olive oil was performed in order to study the centrifugation efficiency to obtain high recovery yield and low co‐extract fat residue in the final extract. Different suitable parameters of MSPD procedure were evaluated, such as nature of dispersing phase, clean‐up adsorbent, and volume of eluting solvent (acetonitrile) in different extraction conditions, with or without sonication. The best results were obtained using 5 g of virgin olive oil, 2 g of PSA as dispersant sorbent, 2 g of Florisil/GCB (70:30 w/w) as clean‐up sorbent, and 15 mL of acetonitrile as eluting solvent under conditions of 15 min ultrasonic bath at RT. Method validation was performed in order to study sensitivity, linearity, precision, and accuracy. Average recoveries ranged between 73.7 and 104.2% with relative SDs 5.3–13.4% at three concentration levels (25, 50, and 100 µg/kg). Detection and quantification limits ranged from 1.5 to 5 µg/kg and 3 to 9 µg/kg, respectively.