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Determination of organophosphorous pesticides in the ppq range using a simple solid‐phase extraction method combined with dispersive liquid–liquid microextraction
Author(s) -
Alves Andreia Cristina Henriques,
Gonçalves Maria Margarida Pontes Boavida,
Bernardo Maria Manuel Serrano,
Mendes Benilde Simões
Publication year - 2011
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.201100434
Subject(s) - chromatography , extraction (chemistry) , chemistry , elution , detection limit , solvent , solid phase extraction , diazinon , tap water , sample preparation , acetone , gas chromatography , pesticide , organic chemistry , environmental engineering , agronomy , biology , engineering
Solid‐phase extraction combined with dispersive liquid–liquid microextraction (SPE‐DLLME) was applied for the extraction of six organophosphorous pesticides (OPPs) in water samples. The analytes considered in this study were determined by gas chromatography with mass spectrometry and included prophos, diazinon, chlorpyrifos methyl, methyl parathion, fenchlorphos and chlorpyrifos. Several extraction conditions (extraction solvent and elution/dispersion solvents nature, extraction solvent volume, elution solvent volume, water volume and sample volume) were tested for SPE‐DLLME with these analytes and the best results were obtained using carbon tetrachloride as the extraction solvent and acetone as the elution/dispersion solvent. Calibration curves for the determination of OPPs in water samples were constructed in the concentration range of 10–100 ng/L. Limits of detection (LODs) ranged from 38 to 230 pg/L values that are below the maximum admissible level for drinking water (100 ng/L). Relative standard deviations (RSD) were between 8.6 and 10.4% for a fortification level of 100 ng/L. At the same fortification level, the relative recoveries (R.R.) of tap, well and irrigation water samples were in the range of 30.2–97.1%.