Binary Dispersive Liquid-Liquid Microextraction Strategy for Accurate and Precise Determination of Micropollutants in Lake, Well and Wastewater Matrices

Bull Environ Contam Toxicol. 2019 Dec;103(6):841-847. doi: 10.1007/s00128-019-02722-x. Epub 2019 Oct 8.


In this study, a binary mixture in dispersive liquid-liquid microextraction was used for the preconcentration and determination of selected pesticides, pharmaceutical and hormone by GC-MS. A Box-Behnken experimental design was used to optimize the amounts of binary mixture, dispersive solvent and salt. The optimum parameters obtained were dichloromethane/1,2-dichloroethane binary mixture (200 µL), ethanol (2.0 mL) and potassium nitrate (1.0 g). Analytical performance of each analyte was determined under the optimum conditions and the lowest and highest detection limits calculated were 0.43 and 5.9 ng/mL. Low relative standard deviations were obtained even in the lowest concentrations in linear calibration plots, signifying high precision for the sample preparation procedure and instrumental measurement. Accuracy of the developed method and applicability to real samples was tested on well, lake, hospital and municipal wastewater. The percent recoveries acquired at different spiked concentrations were satisfactory (89%-108%), validating the accuracy of the method for the quantification of the analytes in the selected matrices.

Keywords: B-DLLME; Experimental design; GC–MS; Pesticide; Wastewater.

MeSH terms

  • Calibration
  • Gas Chromatography-Mass Spectrometry / methods
  • Hormones / analysis
  • Lakes / chemistry*
  • Limit of Detection
  • Liquid Phase Microextraction / methods*
  • Pesticides / analysis
  • Pharmaceutical Preparations / analysis
  • Solvents / analysis
  • Wastewater / analysis
  • Wastewater / chemistry*
  • Water Pollutants, Chemical / analysis*
  • Water Wells*


  • Hormones
  • Pesticides
  • Pharmaceutical Preparations
  • Solvents
  • Waste Water
  • Water Pollutants, Chemical