Rapid separation and highly sensitive detection methodology for sulfonamides in shrimp using a monolithic column coupled with BDD amperometric detection

Talanta. 2009 Sep 15;79(4):1036-41. doi: 10.1016/j.talanta.2009.02.026. Epub 2009 Feb 20.

Abstract

In this report, we aimed to extend our previous efforts toward the evaluation of sulfonamides (SAs) with a boron-doped diamond (BDD) electrode. We improved this method by reducing the analysis time using a monolithic column coupled with amperometric detection to determine seven sulfonamides (sulfaguanidine, sulfadiazine, sulfamethazine, sulfamonomethoxine, sulfamethoxazole, sulfadimethoxine and sulfaquinoxaline). Because of its rapid separation, low back-pressure and high separation efficiency compared to a particle-packed column, a monolithic column (100 mm x 4.6mm) was used for sulfonamide separation. Chromatographic separation was performed in less than 8 min. The analysis was carried out using phosphate buffer (0.1M, pH 3): acetonitrile: methanol in a ratio of 80:15:5 (v/v/v) as the mobile phase with a flow rate of 1.5 mL min(-1). The optimal detection potential using hydrodynamic voltammetry was found to be 1.2V versus Ag/AgCl. The method was applied to determine seven sulfonamides in shrimp after sample preparation by solid-phase extraction. The recoveries of the sulfonamides in spiked shrimp samples at 1.5, 5 and 10 microg g(-1) were in the range of 81.7 to 97.5% with a relative standard deviation (R.S.D.) between 1.0 and 4.6%. Our methodology produced results that were highly correlated with HPLC-MS data. Therefore, we propose a method that can be used for the rapid, selective and sensitive evaluation of sulfonamides in contaminated food.

Publication types

  • Research Support, Non-U.S. Gov't

MeSH terms

  • Animals
  • Boron / chemistry*
  • Chromatography, High Pressure Liquid
  • Diamond / chemistry*
  • Electrochemistry
  • Electrodes
  • Food Analysis / methods*
  • Food Contamination / analysis*
  • Hydrogen-Ion Concentration
  • Mass Spectrometry
  • Penaeidae / chemistry*
  • Reproducibility of Results
  • Shellfish / analysis*
  • Solid Phase Extraction
  • Sulfonamides / analysis*
  • Sulfonamides / chemistry
  • Sulfonamides / isolation & purification
  • Time Factors

Substances

  • Sulfonamides
  • Diamond
  • Boron