| In present work, an efficient, reliable and accurate analytical
method has been used for the extraction of five organophosphorus
pesticides (diazinon, chloropyrifos, phosalone, parathionmethyl and azinphos-methyl) from milk samples. The extracted
analytes were determined with high performance liquid chromatography-diode array detector. For this purpose, the milk proteins are
precipitated by trichloroacetic acid and the analytes dissolved in
the supernatant phase are adsorbed onto an octadecyl silane sorbent. Then, acetone is contacted with the sorbent to elute the
analytes and then it is mixed with toluene. The mixture is rapidly
dispersed into deionised water filled into a syringe. To break down
the obtained cloudy solution, 250 µL acetonitrile is added to the
solution as a demulsifier. Finally, the collected organic phase in the
tip of the syringe is collected, evaporated and reconstituted in
mobile phase for using in determination of the analytes. Figure of
merits were calculated for method validation and acceptable limits
of detection (0.17–0.36 ng mL–1) and quantification (0.57–1.34
ng mL–1), high enrichment factors (395–460) and extraction recoveries (79–92%) were obtained. Inter- (n = 6) and intra-day precisions
at a concentration of 3 ng mL–1 (each analyte) with relative standard deviations ≤7.2%, was obtained. Lastly the method was successfully used for determination of the analytes in some milk
samples and chloropyrifos was found in one sample. |