Salting-out assisted liquid-liquid extraction with the aid of experimental design for determination of benzimidazole fungicides in high salinity samples by high-performance liquid chromatography

Talanta. 2013 Mar 15:106:119-26. doi: 10.1016/j.talanta.2012.12.011. Epub 2012 Dec 14.

Abstract

A novel method for the simultaneous separation and determination of four benzimidazole fungicides (i.e., carbendazim, fuberidazole, thiophanate-methyl and thiophanate) in high salinity samples was developed by using salting-out assisted liquid-liquid extraction (SALLE) via water-miscible acetonitrile as the extractant coupled with high-performance liquid chromatography. Box-Behnken design and response surface were employed to assist the optimization of SALLE conditions, including volume of salting-out solvent, the pH of sample solution and salting-out solvent as variable factors. The optimal salting-out parameters were obtained as follows: 2 mL of acetonitrile was added to 2 mL of sample solution with pH=4 and then 2 mL salting-out solvent containing 5 mol L(-1) sodium chloride at a pH of 7 was added to the solution for extraction. This procedure afforded a convenient and cost-saving operation with good cleanup ability for the benzimidazole fungicides, such as good linear relationships (R>0.996) between peak area and concentration from 2.5 ng mL(-1) to 500 ng mL(-1), low limits of detection between 0.14 ng mL(-1) and 0.38 ng mL(-1) and the intra-day precisions of retention time below 1.0%. The method recoveries obtained at fortified three concentrations for three seawater samples ranged from 60.4% to 99.1%. The simple, rapid and eco-benign SALLE based method proved potentially applicable for trace benzimidazole fungicides analysis in high salinity samples.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Acetonitriles
  • Benzimidazoles / analysis*
  • Carbamates / analysis*
  • Chromatography, High Pressure Liquid
  • Fungicides, Industrial / analysis*
  • Humans
  • Hydrogen-Ion Concentration
  • Limit of Detection
  • Liquid-Liquid Extraction / methods*
  • Reproducibility of Results
  • Salinity
  • Seawater / chemistry
  • Solvents
  • Thiophanate / analogs & derivatives
  • Thiophanate / analysis*
  • Water
  • Water Pollutants, Chemical / analysis*

Substances

  • Acetonitriles
  • Benzimidazoles
  • Carbamates
  • Fungicides, Industrial
  • Solvents
  • Water Pollutants, Chemical
  • Water
  • Thiophanate
  • carbendazim
  • fuberidazole
  • acetonitrile