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Dispersive liquid–liquid microextraction of organophosphorous pesticides using nonhalogenated solvents
Author(s) -
Cristina Henriques Alves Andreia,
Margarida Pontes Boavida Gonçalves Maria,
Manuel Serrano Bernardo Maria,
Simões Mendes Benilde
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.201200241
Subject(s) - chemistry , chromatography , extraction (chemistry) , acetone , detection limit , salting out , solvent , cyclohexane , aqueous solution , organic chemistry
Dispersive liquid–liquid microextraction (DLLME) combined with gas chromatography and mass spectrometry (GC‐MS) was applied to the determination of five organophosphorous pesticides (OPPs) in water samples. The analytes included in this study were prophos, diazinon, chlorpyrifos methyl, fenchlorphos, and chlorpyrifos. The use of nonhalogenated solvents (cyclohexane, heptane, and octane) as extraction solvents was investigated using acetone, acetonitrile, or methanol, as dispersion solvents. The combination of less polar dispersion solvents (1‐propanol and 2‐propanol) and nonhalogenated extraction solvents was also studied in dispersive liquid–liquid microextraction for the first time. Several experimental conditions were tested (nature and volume of extraction solvents, nature and volume of dispersion solvents, salting‐out effect) and the corresponding enrichment factors and recoveries were evaluated. The best microextraction condition was obtained using 50 μL of cyclohexane and 0.3 mL of 1‐propanol. The detection and quantification limits were in the low ppt range, with values between 3.3–8.0 ng/L and 11.0–26.6 ng/L, respectively. Relative standard deviations were between 6.6 and 13.1% for a fortification level of 500 ng/L. At the same fortification level, the relative recoveries (RR) of Alvito's dam water, Judeu's river water, and well water samples were in the range of 50.3–97.1%.