One-pot synthesis of a multi-template molecularly imprinted polymer for the extraction of six sulfonamide residues from milk before high-performance liquid chromatography with diode array detection

J Sep Sci. 2018 Feb;41(3):723-731. doi: 10.1002/jssc.201701205. Epub 2017 Dec 18.


A highly selective molecularly imprinted polymer sorbent was synthesized and employed for the simultaneous determination of six sulfonamide antibiotic residues (sulfanilamide, sulfacetamide, sulfadiazine, sulfathiazole, sulfamerazine, and sulfamethizole) in milk samples. Multi-analyte imprinted particles were used as a sorbent in solid-phase extraction. Sulfonamides were separated on a high-performance liquid chromatography column (Merck-Lichrospher RP18e, 5 μm 250 × 4 mm) and further identified and quantified by diode array detection. Several parameters including required loading of the molecularly imprinted polymer sorbent, mass of milk, volume, and type of elution solvent, as well as time for absorption and elution were investigated to obtain optimal experimental conditions. For comparison purpose, a non-imprinted polymer was applied under the optimum conditions. The validation study according to the European Union Decision 2002/657/EC was based on the investigation of linearity, selectivity, stability, limits of detection and quantitation, decision limit, detection capability, trueness, precision, and ruggedness according to Youden's approach. The decision limit and detection capability values in the milk were achieved from 101.9 to 113.5 μg/kg and from 114.4 to 135.4 μg/kg, respectively, depending on the target sulfonamide drug. Finally, the optimized protocol was successfully applied to commercial milk samples and human breast milk.

Keywords: milk; multi-template molecularly imprinted polymers; sol-gel processes; solid-phase extraction; sulfonamide drugs.

MeSH terms

  • Animals
  • Anti-Bacterial Agents / analysis
  • Chromatography, High Pressure Liquid*
  • Food Analysis / methods*
  • Food Contamination / analysis*
  • Humans
  • Milk / chemistry*
  • Milk, Human / chemistry*
  • Molecular Imprinting
  • Polymers / analysis
  • Polymers / chemical synthesis*
  • Reproducibility of Results
  • Solid Phase Extraction
  • Solvents
  • Sulfonamides / analysis*


  • Anti-Bacterial Agents
  • Polymers
  • Solvents
  • Sulfonamides