a LC–MS system (Agilent 1260/6150B, Agilent Technologies, USA)
equipped with a Zorbax Eclipse plus C18 column (4.6 × 150 mm
and 3.5 μm dia, Agilent Technologies, USA). The oven temperature
was maintained at 35 °C throughout the analysis. The mobile phases
were 10 mM aqueous ammonium acetate solution (A) and methanol (B).
The mobile phase gradient started at 70% B at 0.0 → 3.0 min,
and went to 95% B at 3.0 → 6.0 min and then 70% B at 6.0 min
following post-run time of 5.0 min with the flow rate set at 0.5 mL
min–1. The analysis was done in the negative mode
with the single quadrupole mass spectrometer and other set parameters
were: drying gas flow 12.0 mL min–1 at 300 °C,
nebulizer pressure 35 psi, capillary voltage 4000 V, SIM ion 219 →
221 amu, fragmentor voltage 100 V, and sheath gas flow 3.0 mL min–1 at 150 °C. The data obtained were processed
using Agilent OpenLAB CDS ChemStation software. The standard curve
was linear over the tested concentration range (R2, 0.998). The LOD and LOQ values were 0.007 and 0.03
mg L–1, respectively. The recovery (mean, n = 3) of spiked 2,4-D for 0.031–0.5 mg L–1 ranged between 87.98 and 117.94%. Therefore, the method appears
to be reliable and accurate for the determination of the 2,4-D in
different urban soils.