| A rapid, efficient and reliable microwave-assisted homogenous
liquid–liquid microextraction method has been developed for the
extraction of pyrethroid pesticides from fresh fruit and vegetable
samples prior to their determination by gas chromatography–mass
spectrometry. For this purpose, first, the samples are crushed and
the obtained juices are separated and transferred into a glass test
tube. Then, a mixture of methanol and deionised water is used to
extract the analyte residues in refuse of the samples. The supernatant phase is removed and mixed with the related juice obtained
from the previous step. After that, the solution temperature is
adjusted at −10°C and a few microlitres of chloroform is dissolved
in it. Then, it is exposed to microwave irradiations to break down
the homogenous phase. In this step, a cloudy state is produced and
the tiny droplets of chloroform containing the extracted analytes
are sedimented at the bottom of the tube. A portion of the sedimented phase is removed and injected into the separation system.
Validation of the method showed that limits of detection and
quantification were in the ranges of 4.3–9.4 and 14.4–30.5 ng kg−1
,
respectively. Enrichment factors and extraction recoveries of the
selected analytes ranged from 315 to 415% and 63–83%, respectively. The method had a proper precision with relative standard
deviations less than ≤7.7% for intra-(n = 6) and inter-day (n = 6)
precisions at a concentration of 75 ng kg−1 of each analyte. Finally,
the method was used for determination of the analytes in fresh fruit
and vegetable samples in a predetermined times. |