Rapid determination of antibiotic residues in cereals by liquid chromatography triple mass spectrometry

Anal Bioanal Chem. 2019 Sep;411(23):6129-6139. doi: 10.1007/s00216-019-02003-w. Epub 2019 Jul 5.

Abstract

Antibiotics may be present in agricultural soils through the application of organic amendments as fertilizers or by irrigation of fields with recycled water. As a result of these agricultural practices, antibiotics in soil can lead to their uptake by plants, entering in this way the food chain. Studies on the levels of antibiotics in cereal samples are scarce in the available literature. In this work, an analytical method was developed for the determination of 19 antibiotics (fluoroquinolones, sulfonamides, tetracyclines, and lincosamides) in four types of cereal grains (wheat, barley, rice, and oat). Ultrasound-assisted matrix solid-phase dispersion was selected as extraction technique with recoveries of target analytes ranging from 73 to 127% for the four cereals analyzed. Limits of quantification obtained ranged from 0.8 to 5.8 ng g-1. Compared with methods described for the analysis of antibiotics in cereals, the developed method uses a lower volume of extraction solvent and very good recoveries were obtained for all compounds. The validated method was applied to the analysis of different types of cereals samples, harvested from agricultural fields or purchased from local supermarkets. The analysis of the five cereal samples grown in fields with 3 years of consecutive organic amendments revealed that none of the nineteen antibiotics selected were found in any sample. Eleven commercial samples of cereals of different types and presentations were analyzed and enrofloxacin was detected in one rice sample; the presence of enrofloxacin in cereals or its incorporation into crops from soil or water not previously reported. Graphical abstract.

Keywords: Analysis; Antibiotics; Grains; LC-MS/MS; Uptake.

Publication types

  • Validation Study

MeSH terms

  • Anti-Bacterial Agents / analysis*
  • Chromatography, Liquid / methods
  • Drug Residues / analysis*
  • Edible Grain / chemistry*
  • Fluoroquinolones / analysis
  • Food Contamination / analysis*
  • Limit of Detection
  • Lincosamides / analysis
  • Solid Phase Extraction / methods
  • Sulfonamides / analysis
  • Tandem Mass Spectrometry / methods*
  • Tetracyclines / analysis

Substances

  • Anti-Bacterial Agents
  • Fluoroquinolones
  • Lincosamides
  • Sulfonamides
  • Tetracyclines