Sensitive Determination of Acetochlor, Alachlor, Metolachlor and Fenthion Utilizing Mechanical Shaking Assisted Dispersive Liquid-Liquid Microextraction Prior to Gas Chromatography-Mass Spectrometry

Bull Environ Contam Toxicol. 2020 Sep;105(3):460-467. doi: 10.1007/s00128-020-02965-z. Epub 2020 Aug 24.

Abstract

A green, sensitive and accurate dispersive liquid-liquid microextraction (DLLME) method was used to preconcentrate four selected pesticides in dam lake water samples for determination by gas chromatography-mass spectrometry (GC-MS). Conditions of the DLLME method were comprehensively investigated and optimized according to type/volume of extraction solvent, type/volume of dispersive solvent, and type/period of mixing. The developed method was validated according to the limits of detection and quantitation, accuracy, precision and linearity. Under the optimum conditions, limit of detection values calculated for alachlor, acetochlor, metolachlor and fenthion were 1.7, 1.7, 0.2 and 7.8 µg/kg (mass based), respectively. The method recorded 202, 104, 275 and 165 folds improvement in detection power values for acetochlor, alachlor, metolachlor and fenthion, respectively, when compared with direct GC-MS measurements. In order to evaluate the accuracy of the developed method, real sample application with spiking experiments was performed on dam lake water samples, and satisfactory percent recovery results in the range of 81%-120% were obtained.

Keywords: DLLME; GC–MS; Herbicides; Insecticide; Water quality.

MeSH terms

  • Acetamides / analysis
  • Fenthion / analysis
  • Fresh Water / chemistry
  • Gas Chromatography-Mass Spectrometry / methods
  • Limit of Detection
  • Liquid Phase Microextraction / methods*
  • Pesticides / analysis*
  • Solvents / analysis
  • Toluidines / analysis
  • Water Pollutants, Chemical / analysis*

Substances

  • Acetamides
  • Pesticides
  • Solvents
  • Toluidines
  • Water Pollutants, Chemical
  • alachlor
  • acetochlor
  • Fenthion
  • metolachlor