Method optimization and validation for the determination of eight sulfonamides in chicken muscle and eggs by modified QuEChERS and liquid chromatography with fluorescence detection

J Pharm Biomed Anal. 2016 May 30:124:261-266. doi: 10.1016/j.jpba.2016.02.040. Epub 2016 Mar 3.

Abstract

A simple, effective and reliable method for the determination of eight sulfonamide antibiotics (sulfadiazine, sulfapiridine, sulfamerazine, sulfamethazine, sulfachloropiridazine, sulfamethoxazole, sulfadoxine, sulfadimethoxin) in chicken muscle and eggs by liquid chromatography and fluorescence detection has been developed and validated. Sulfonamides do not present native fluorescence, however their direct determination was achieved by on-line post-column photochemical derivatization by UV irradiation. Sample treatment was based on QuEChERS with several modifications depending on the matrix. Egg extracts were cleaned-up using PSA for the dispersive solid phase extraction step. On the other hand, a new clean-up sorbent, Supel™ QuE Z-Sep(+), has been successfully applied in chicken muscle extract and has proved to be effective for interference removal from this matrix. Under optimum conditions, recoveries from 65.9 to 88.1%, relative standard deviations lower than 10% (except for sulfachloropiridazine), and limits of quantification (LOQs) from 14 to 85 μg kg(-1) were achieved. Thus, the method complies with current European requirements.

Keywords: Egg; HPLC; Meat; Photoinduced fluorescence; QuEChERS; Sulfonamides.

Publication types

  • Research Support, Non-U.S. Gov't
  • Validation Study

MeSH terms

  • Animals
  • Calibration
  • Chickens
  • Chromatography, Liquid / methods*
  • Eggs / analysis*
  • Limit of Detection
  • Muscles / chemistry*
  • Reproducibility of Results
  • Spectrometry, Fluorescence / methods*
  • Sulfonamides / analysis*

Substances

  • Sulfonamides