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Vortex‐assisted liquid–liquid microextraction combined with gas chromatography‐mass spectrometry for the determination of organophosphate pesticides in environmental water samples and wines
Author(s) -
Zacharis Constantinos K.,
Christophoridis Christophoros,
Fytianos Konstantinos
Publication year - 2012
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201200309
Subject(s) - chromatography , chemistry , extraction (chemistry) , toluene , solvent , gas chromatography , detection limit , enrichment factor , mass spectrometry , gas chromatography–mass spectrometry , sample preparation , pesticide , organic chemistry , agronomy , biology
A simple vortex‐assisted liquid–liquid microextraction protocol followed by GC ‐ MS is proposed for the determination of 12 organophosphate pesticides residues in environmental water samples and wines. The sample pretreatment employs the usage of low‐density organic solvent. The parameters affecting the extraction efficiency (type and volume of organic extraction solvent, sample pH, ionic strength, extraction time, and centrifugation speed) were carefully examined. A mild emulsification process was involved by the addition of 40 μL toluene into 10 mL sample followed by sequential vortex‐based agitation and manual shaking for 3 min. Following the extraction, the pesticide‐rich organic solvent was recovered by centrifugation at 4000 rpm for 5 min. A fraction of the floated toluene was then collected and analyzed by GC ‐ MS in SIM mode. Under the optimized conditions, the enrichment factor ranged between 65 and 389. Satisfactory linearity was observed for all pesticides tested with correlation coefficients higher than 0.9945 while the LOD s were in the range of 2–11 ng L −1 . The main advantages of the proposed method are the simplicity of operation, rapidity, low cost, and high sensitivity.