Determination of Commonly Used Herbicides in Surface Water Using Solid-Phase Extraction and Dual-Column HPLC-DAD

The present study describes the application of different solid-phase extraction techniques for the extraction, separation, and quantitative determination of 10 commonly used herbicides with different chemical structures (chlorsulfuron, diuron, bentazone, linuron, chlorpropham, fenoxoprop-ethyl, MCPA, diclofop-methyl, fluazifop-butyl, trifluraline) in water. Octadecyl (C₁₈) Empore extraction disks, octadecyl (C₁₈), and stryene divinylbenzene (SDB) Bond Elut Env cartridges were compared for solid-phase extraction efficiency. Herbicides were separated and quantified by reversed-phase high performance liquid chromatography with diode-array detection (HPLC-DAD) with simultaneous separation on two columns of differing polarity (C₁₈ and CN) to confirm identification. Analytical separation was performed simultaneously on C₁₈ and CN columns. Reanalysis of the sample extracts on a (cyano) CN column were used to confirm the identity of these compounds. Method optimization and validation parameters were presented in this work. Recoveries varied from 76.0% to 99.0% for C₁₈ disks, from 75.1% to 100.0% for C₁₈ cartridges, and from 54.0% to 98.0% for SDB cartridges over concentrations at 0.025–0.4 μg L⁻¹. The limits of detection were 0.012–0.035 μg L⁻¹.

Key Words:

• HPLC-DAD
• Solid-phase extraction
• Water analysis
• Method development
• Herbicides.

ACKNOWLEDGMENTS

This work was supported by the Research Fund of Istanbul University (1758/21122001).

Notes

^aMCPA: 4-Chloro-2-methyl-phenoxyacetic acid.